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Page 1: PROGRAM & ABSTRACT BOOK - utm.my . Assalamualaikum and Salam Sejahtera . I am pleased to welcome all participants to MySSC2017, organized by the Faculty of Science, Universiti Teknologi

PROGRAM & ABSTRACTBOOK

Page 2: PROGRAM & ABSTRACT BOOK - utm.my . Assalamualaikum and Salam Sejahtera . I am pleased to welcome all participants to MySSC2017, organized by the Faculty of Science, Universiti Teknologi

CONTENT

FOREWORD 2

ORGANIZING COMMITTEE 4

CONFERENCE PROGRAM 5

LOCATION AND MAP OF PULAI SPRINGS RESORT 8

ABSTRACTS

PLENARY LECTURE 9

KEYNOTE LECTURE 9

INVITED LECTURE 10

ORAL PRESENTATION 13

POSTER PRESENTATION 22

SPONSORS 28

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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FOREWORD

Assalamualaikum and Salam Sejahtera

Welcome to the first Malaysia Separation Science Conference 2017 (MySSC 2017)

held on 23rd - 25th October 2017 at Pulai Springs Resort, Johor Bahru, Johor, Ma-

laysia. This Separation Science Conference has been mooted for quite some time

and we are delighted with the outcome of MySSC 2017. Universiti Teknologi Ma-

laysia (UTM) is honoured to host this flagship event in close collaboration with the

American Chemical Society (ACS) Malaysia Chapter, Malaysian Analytical Sciences Society (ANALIS)

and Forensic Science Society of Malaysia (FSSM). We hope that MySSC2017 will pave the way to a

more successful MySSC in the future.

At this juncture, we are harbouring on the idea of initiating the foundation of the Malaysia Separation

Science Society (MySSS). Furthermore, we are also eyeing on strategic collaborations and networking

not only within Malaysia, but also between neighbouring countries such as Indonesia, Thailand and

Singapore with the possibility of future involvement of other countries.

My deepest appreciation goes to the plenary speaker, keynote speakers and presenters for their com-

mitment to participate in MySSC2017 and to share their expertise and experiences in their respective

fields with all the participants, especially the young researchers. MySSC will serve as a platform for

academicians, scientists, researchers and students in the field of separation science to share recent

research findings, exchange ideas and knowledge on the latest development and advancement, and

to encourage the development of professional and social networking amongst the participants. The

theme of MySSC2017 is Towards Sustainable Innovation. Active collaboration with various stakehold-

ers throughout society (trans-disciplinary) must form another critical component of sustainability sci-

ence.

We are delighted in organizing this conference that allows multidisciplinary individuals to interact and

share their knowledge even for a short period of time. We would also like to commend the effort of

Faculty of Science, UTM for facilitating this congregation of researchers. I believe that this event in

this region will produce both positive environmental and economical benefits for all of us.

I wish to express my gratitude and appreciation to UTM, ACS Malaysia Chapter, ANALIS and FSSM and

also to all our sponsors for the financial support in making MySSC2017 a reality. Also, I would like to

take this opportunity to thank all the committee members for their hard work in ensuring the success

of MySSC 2017. Without the cooperation and collaborating teamwork, MySSC2017 will not be real-

ized. I am happy to see delegates from Thailand, Taiwan and Indonesia coming to MySSC 2017. To all

our presenters and participants, enjoy Johor Bahru, the beautiful capital of Johor. Have an enjoyable,

fruitful and memorable moments.

PROFESSOR DR. WAN AINI WAN IBRAHIM (FMIC) CHAIRPERSON MySSC2017

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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Page 4: PROGRAM & ABSTRACT BOOK - utm.my . Assalamualaikum and Salam Sejahtera . I am pleased to welcome all participants to MySSC2017, organized by the Faculty of Science, Universiti Teknologi

FOREWORD

Assalamualaikum and Salam Sejahtera

I am pleased to welcome all participants to MySSC2017, organized by the Faculty

of Science, Universiti Teknologi Malaysia. This conference provides a platform for

researchers to interact and form collaborations in the field of separation science,

be it in the development or the processes. It is with high hope that this meeting of

scientific minds will be fruitful, leading to the formation of efficient and strong na-

tional, regional and international networks.

I hope that the primary aim of this conference that is to develop fundamental understanding and

application of key aspects in separation science can be achieved successfully. With UTM’s research

strength and innovation, the conference can push forward the efforts to establish links between re-

cent advancements in the science academic fields and the business industries. Such outcome could

create various values and opportunities for researchers and their products in benefitting Malaysia’s

research agenda. I have always believed that a technologically literate scientific community with high

awareness towards the importance of the advancement of knowledge and skills related to separation

science is essential for high value added enterprises to ensure the sustainability in the quality of life

with safer, cleaner and healthier environment.

I sincerely hope that this conference will bring together researchers and scholars from different fields

of separation science to share their views and experiences, and thus enriching the knowledge and

quality of research in this important field. The invaluable exchange of ideas and the forging of net-

works between participants during conferences like this may not be possible if not for the Government

and Private Sector fundings of Research Grants. Therefore, I hope that more research grants can be

secured as a consequence of this conference.

PROFESSOR DR. NORSARAHAIDA S. AMIN

Dean, Faculty of Science

Universiti Teknologi Malaysia

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ORGANIZING COMMITTEE

Prof. Dr. Wan Aini Wan Ibrahim Chairperson

Prof. Dr. Mohd Marsin Sanagi Co-Chair

Dr. Aemi Syazwani Abdul Keyon Secretariat

Assoc. Prof. Dr. Azli Sulaiman Treasurer

Dr. Hasmerya Maarof Head of ICT & Promotion

Prof. Dr. Sugeng Triwahyono Head of Scientific Committee

Dr. Khairil Juhanni Abdul Karim Head of Sponsorship & Gift Committee

Dr. Naji Arafat Mahat Head of Technical & Workshop Committee

Dr. Umi Kalthom Ahmad Head of Protocol and Logistics Committee

COMMITTEE MEMBERS

Assoc. Prof. Dr. Zainab Ramli

Dr. Susilawati Toemen

Dr. Shajarahtunnur Jamil

Dr. Norazah Basar

Dr. Sheela Chandren

Dr. See Hong Heng

Dr. Che Rozid Mamat

Mohd. Daniel Abdullah

Hashim Baharin

Azani Ishak

Fuaad Omar

Nurul Hajar Sapiren

Zarina Junet

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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CONFERENCE PROGRAM

Plenary, Keynote, Invited and Oral presentations are each allocated with 60, 45, 30 and 20 minutes, respectively

including Q&A session. For poster presentation, the poster type will be A1 size. Posters should be put up through-

out the presentation day and immediately removed prior to closing ceremony.

23 October 2017

Pre-Conference Workshop

09.00 – 12.00 “Mass Spectrometry Seminar” Presenter: Agilent Technologies Venue: Maharaja Room, Pulai Springs Resort

14.00 – 17.00 “Mass Detection Educational Workshop” Presenter: Waters Analytical Instrument Venue: Maharaja Room, Pulai Springs Resort

08.30 – 17.00 “Chemometrics Made Easy” Venue: Bilik Mesyuarat Jab. Kimia 2F, C10 Building, UTM Johor Bahru, Johor

24 October 2017

(Venue: Inderaputera Room)

08.00 – 08.50 Registration

08.50 – 09.00 Welcome Speech

09.00 – 10.00

Plenary 1 : Lee Hian Kee “From Learning To Walk To Running Uninterruptedly: The Road To Developing An Automated Integrative Analytical Platform” Chairperson : Mohd Marsin Sanagi

10.00 – 10.15 Coffee Break (Venue: Ramayana)

10.15 – 11.15 Plenary 2 : Joselito P. Quirino “New Uses Of Cyclodextrins For Separation Science” Chairperson : Baharuddin Saad

11.15 – 11.30 Group Photo Session

Chairperson : Jen-Fon Jen/Hasmerya Maarof

11.30 – 12.00 Invited 1 : Marinah Mohd Ariffin* And Nurul Ashikin Binti Mohyidin “Molecularly-Imprinted Polymer Solid-Phase Extraction For Determination Of Atrazine In Soil Samples”

12.00 – 12.20

Oral 1 : Syazwani Binti Dzolin, Wan Aini Wan Ibrahim and Naji Arafat Mahat “Ulti-Trace Metals Fingerprinting Of Peninsular Malaysia Stingless Bee Honeys From Different Regions And Seasons Using Inductively Coupled Plasma Optical Emission Spectrometry And Chemometric Techniques”

12.20 – 12.40

Oral 2 : Ahmad Anwarud Dawam, Yatim Lailun Ni’mah, Ratna Ediati, Didik Prasetyoko, Sugeng Triwahyono, Aishah Abdul Jalil “Red Mud As Alumina Source In The Synthesis Of Mesoporous Aluminosilicate And Its Application As Catalyst Esterification Of Reutalis Trisperma Oil”

12.40 – 13.00 Oral 3 : Fathiah Ahmad Zubaidi “Robust And High Throughput Fia-Ms3 Spectrometry For The Differentiation Of Isomeric Compounds In Dried Blood Stain-Application To Forensic Toxicology Cases In Malaysia”

13.00 – 14.00 Lunch Break (Venue: Gleneagles Terrace)

14.00 – 14.30 Poster Session

Chairperson : Basuki Wirjosentono/Susilawati Toemen

14.30 – 15.00 Invited 2 : Aishah A. Jalil “Electrochemical-Induced Synthesis Of NiAl2O4/Al2O3 For Adsorption Of Pd(II)”

15.00 – 15.30

Invited 3 : Norfarah Syuhaidah Mohd Noor, Nik Ahmad Nizam Nik Malek*, Noor Asyraf Noor Azman, Muhammad Arshad Javed “Surfactant Modified Zeolite With Ammonium, Phosphate And Potassium As Regenerated Controlled Release Fertilizer”

15.30 – 15.50 Oral 4 : Sri Setyaningsih, I. Qoniah, Meyga Evi Ferama Sari, Ratna Ediati, Didik Prasetyoko “Effect Of Crystallization Times On Synthesis Of Zeolite Afrom Volcanic Sand Of Kelud Volcano”

15.50 – 16.10 Oral 5 : Vita Nur Iftitahiyah, Didik Prasetyoko, Hartati, Yatim Nailun Nikmah, Hadi Nur “Esterification Of Acetic Acid And Benzyl Alcohol Over Zeolite HX From Bangka Belitung Kaolin”

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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16.10 – 16.30 Oral 6 : Nur Fatihah Tajul Arifin, Madzlan Aziz “Preparation And Characterization Of Improved Hydrophilic Polyethersulfone/Reduced Graphene Oxide Membrane”

16.30 – 17.00 Discussion on collaboration and formation of Malaysia Separation Society

17.00 – 17.15 Coffee Break (Venue: Ramayana)

20.00 – 22.00 DINNER & OPENING CEREMONY Venue: Kayangan Suites

25 October 2017 (Venue: Inderaputera Room)

Chairperson : Naji Arafat Mahat/Sheela Chandren

08.30 – 08.50 Oral 7 : Zanariah Hashim, Tairo Ogura and Eiichiro Fukusaki “Accelerated Ion-Pair Lc-Ms/Ms For High Throughput Metabolite Profiling”

08.50 – 09.10

Oral 8 : Choong Yew Keong, Nor Syaidatul Akmal Mohd Yousof, Mohd Isa Wasiman, Jamia Azdina Jamal, Zhari Ismail “Development Of Ftir Database Of Roselle Raw Material Originated From Western Coastline In Peninsular Malaysia”

09.10 – 09.30 Oral 9 : K. Bachuri, Mariya Tijjani, Anthony Nyangson Steven, Nur Izzati Mohd Noh “Identification Of Flavonoids Biosynthesis By An Indigenious Herbal Plant From Borneo Island”

09.30 – 10.00 Invited 4 : Ku Madihah K.Y., Zaibunnisa A.H, Osman, R., Misnawi. J., Norashikin Saim “Discrimination Between Arabica And Robusta Coffee Beans Using Flavor Compounds”

10.00 – 10.30 Invited 5 : Ida Idayu Muhamad “Greener, Nutritious Seed Oils From Microwave-Assisted Aqueous Enzymatic Extraction“

10.30– 10.45 Coffee Break (Venue: Ramayana)

Chairperson : Joselito P. Quirino/Khairil J. Abdul Karim

10.45 – 11.30 Keynote 1 : Baharuddin Saad and Nor Shifa Shuib “Green Methods For The Determination Of Aflatoxins”

11.30 – 12.00 Invited 6 : Basuki Wirjosentono, Tamrin, Pevi Riani, Ridwanto, Eddyanto, Ahmad Nasir Pulungan, Sunit Hendrana, Diana Adnanda Nasution, Hanafi Ismail, I Putu Mahendra “Processings And Characterisations Of Polymeric Materials For Separation Processes”

12.00 – 12.20 Oral 10 : Boon Yih Hui, M. Raoov, N. N. M. Zain, S. Mohamad and H. Osman “Magnetic Solid-Phase Extraction Using Fe3o4@Ionic Liquid-Β-Cyclodextrin Polymer As Adsorbents For Analysis Of Aromatic Amines Coupled With Gc-Fid”

12.20 – 12.40 Oral 11 : Faridah Mohd Marsin, Wan Aini Wan Ibrahim, Hamid Rashidi Nodeh, Mohd Marsin Sanagi “Preparation Of Ternary Oil Palm Empty Fruit Bunch Activated Carbon- Magnetite-Polypyrrole For The Extraction Of Endosulfan And Dieldrin Using Response Surface Methodology”

12.40 – 13.00 Oral 12 : Abdulaziz Mohd. Hassan, Wan Aini Wan Ibrahim, Mohd Bakri Bakar, Mohd Masin Sanagi “New 3-Aminopropyltrimethoxysilane Functionalized Magnetic Sporopollenin-Based Graphene Oxide Adsorbent For Removal Of Pb(Ii) From Aqueous Solution”

13.00 – 14.00 Lunch Break (Venue: Gleneagles Terrace)

14.00 – 14.30 Poster Session

Chairperson : Azli Sulaiman/Sugeng Triwahyono

14.30 – 15.00 Invited 7 : Hasmerya Maarof “Role Of Molecular Modelling To Enhance The Understanding Of Separation Science Study“

15.00 – 15.30

Invited 8 : Dadan Hermawan, Uyi Sulaeman, Suwandri, Asmiyenti Djaliasrin Djalil, Hassan Y. Aboul-Enein “Application Of Chiral And Non-Chiral HPLC Method For Selected Antifungal Drug Analysis In The Pharmaceutical Formulation”

15.30 – 15.50 Oral 13 : Nurul Raihana Binti Azhari, M. Raaov, N. Yahaya, F. B. M. Suah “Enantiomeric Resolution Of Imidazole Antifungal Agents Using Different Modified Cyclodextrins As Chiral Selectors In Capillary Electrophoresis.”

15.50 – 16.10

Oral 14 : Nurzaimah Binti Zaini @ Othman, Nor Suhaila Mohamad Hanapi, Wan Nazihah Wan Ibrahim And Nor’ashikin Saim “Selective Determination Of Acidic Drugs In Water Samples By On-Line Solid Phase Extraction Liquid Chromatography Using Alginate Incorporated MultiWalled Carbon Nanotubes As Sorbent”

16.10 – 16.30

Oral 15 : Mohammad Salim Tabish, Nor Suhaila Mohamad Hanapi, Nor’ashikin Saim And Wan Nazihah Wan Ibrahim ”Micro-Solid Phase Extraction Using Alginate/Graphene Oxide (Alg-Go) For The Determination Of Selected Non-Steroidal Anti-Inflammatory Drugs From Water Samples”

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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16.30 – 16.50 Oral 16 : Siti Munirah Abd Wahib, W. A. Wan Ibrahim And M. M. Sanagi “Eco-Friendly Magnetic Adsorbent For Dispersive Micro-Solid Phase Extraction Of Non-Steroidal Anti-Inflammatory Drugs From Aqueous Samples”

16.50 – 17.10 Oral 17 : Miftakhul Jannatin, Ganden Supriyanto, Pratiwi Pudjiastuti, Wan Aini Wan Ibrahim “Complex Reaction Of Histamine, Metal And Alizarin Red S As A Novel Spectrophotometric Method For Histamine Determination In Fish”

17.10 – 17.25 CLOSING CEREMONY & COFFEE BREAK

POSTER PRESENTATION

P01 C. Ratchanee, S. Naphapob, T. Parinya And P. Atikorn “Physico-Chemical And Functional Properties Of Rice Bran Protein Hydrolyzed And Their Application In Food Model”

P02 S. Eadmusik, C. Phungamngoen And N. Choosuk ”Kinetic Degradation Of Total Phenolic Content, Dpph Radicle Scavenging Activity And Xanthine Oxidase Inhibitory Activity In Yanang (Tiliacora Triandra) Leaf Extract”

P03 Natthaya Choosuk, Nattakan Jakkranuhwat, Chanthima Phungamngoen, Patcharee Kunchansombat “Effect Of Pre-Treatment On The Quality Of Dried Coconut During Storage”

P04 S. Tipkanon, R. Charoen, W. Savedboworn And W. Riansa-Ngawong “Optimization Of Herbal Health Tea Flavored With Roasted Rice Germ (Khao Dawk Mali 105) Using Response Surface Methodology”

P05 P. Renumarn, K.K. Joachim, C. Phungamngoen And N. Choosuk

“Effect Of Pre-Treatments On Qualities Of Minimally Processed Shallots (Allium Ascalonicum L.)”

P06 Othman, A. Sulaiman And I. Ibrahim

“The Use Of Low Grade Limestone In Acid Mine Drainage Treatment”

P07 Husnul Hanani Soib, Harisun Yaakob, Mohamad Roji Sarmidi, Mohamad Norisham Mohamad Rosdi “Fractionation Of Aqueous Extract Of Ficus Deltoidea Var. Kunstleri’s Leaves Using Solid Phase Extration Method For Anticancer Activity On Du145 Cell Line ”

P08 H.-K. Shih, C.-W. Lin, J.-F. Jen “Eco-Friendly Analysis Of Parabens In Cosmetics By In-Tube Salt-Assisted Homogeneous Liquid-Liquid Extraction And Subcritical Water Chromatography With Ultraviolet Detection”

P09 Faridah Mohd Marsin, Wan Aini Wan Ibrahim, Hamid Rashidi Nodeh, Mohd Marsin Sanagi

”Optimization Of The Preparation Of Ternary Magnetite-Graphene Oxide-Polypyrrole Nanocomposite For The Extraction Of Imidacloprid Using Response Surface Methodology”

P10 S. Triwahyono, A.A. Jalil And N. Salamun

“Zirconium Loaded Mesostructured Silica Nanoparticles Adsorbent For Removal Of Hexavalent Chromium From Aqueous Solution”

P11 Susilawati Toemen, Wan Azelee Wan Abu Bakar, Salmiah Jamal Mat Rosid And Wan Nur Aini Wan Mokhtar “Analysis Of Structure-Activity Relationships Of CO2 Methanation Reaction Over Caria Based Catalysts”

P12 Khairunnabihah Bachuri, Nur Izzati Mohd Noh, Anthony Nyangson Steven ”Identification Of Anti-Cancer Agents In An Indigenous Plant Using UHPLC-Ms/Ms”

P13 Norazah Basar, Nurshahira Mohd Rozi “Quantification Of Flavonoids From Leaves Of Moringa Oleifera Lam”

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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LOCATION AND MAP OF PULAI SPRINGS RESORT

Jalan Pontian Lama, 81110 Johor, Malaysia

Phone: +60 7-521 2121

(Latitude, Longitude)

(1.554453200, 103.612999300)

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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PLENARY LECTURE

FROM LEARNING TO WALK TO RUNNING UNINTERRUPTEDLY: THE ROAD TO

DEVELOPING AN AUTOMATED INTEGRATIVE ANALYTICAL PLATFORM

Lee Hian Kee

Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543

National University of Singapore Environmental Research Institute

T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411

The advantageous capabilities of miniaturized sample preparation approaches such as solid-phase microextraction

(SPME) and liquid-phase microextraction (LPME) render them eminently suitable for automation. In the case of

SPME, modern autosampling instrumentation permitting its automation has been available for many years, and

related sorbent-based procedures such as stir-bar sorptive extraction, disposable pipette extraction and microex-

traction by packed sorbent, etc. have followed suit. Apart from single-drop microextraction which can be auto-

mated using currently commercially available autosamplers due to the simplicity of the procedure, LPME-based

automation has been very rare. For the past several years we have been working on the development of LPME-

based techniques automation by making the most of off-the- shelf commercial equipment, rather than trying to

tailor-make experimental setups and assemblies from different components, with all their attendant inconven-

iences, for the same purpose. We have been attempting to set up fully-automated analytical platforms comprising

not only sample preparation seamlessly coupled to analytical systems (primarily chromatography) but also to the

front-end of the workflow, i.e., (water) sampling, based on originally manual LPME procedures. In this talk, we

shall describe some of these developments that have the potential to be applied remotely from the conventional,

fixed-location laboratory, in effect making the environment an onsite laboratory.

--oOo--

NEW USES OF CYCLODEXTRINS FOR SEPARATION SCIENCE

Joselito P. Quirino

Room 2026, Chemistry Building, Sandy Bay Campus, University of Tasmania, Tasmania, Australia

Cyclodextrins (CDs) belongs to a group of cyclic oligosaccharides with (1-4) ether linkages of glucopyranose

units. They have the shape of a truncated cone, with the internal cavity showing a hydrophobic character while

the external surfaces are hydrophilic [1]. The great interest on CDs is primarily due to the ability of the CD’s

cavity to include a wide range of guest molecules, including surfactants. The cavities also impart enantioselectiv-

ity, which is the fundamental basis of the wide use of CDs in chiral separations by chromatography or capillary

electrophoresis (CE) [2,3]. In this talk, new and unique uses of CDs for separation science will be presented.

[1] A. J. M. Valente, O. Söderman, Adv. Colloid Interface Sci. 2015 (2014) 156-176.

[2] J. M. Saz, M. L. Marina, J Chromatogr. A 1467 (2016) 79-94.

[3] M. Silva, D. Pérez-Quintanilla, S. Morante-Zarcero, I. Sierra, M. L. Marina, Z. Aturki, S. Fanali, J Chroma-

togr. A 1490 (2017) 166-176.

--oOo--

KEYNOTE LECTURE

GREEN METHODS FOR THE DETERMINATION OF AFLATOXINS

Bahruddin Saad* and Nor Shifa Shuib1

*Fundamental and Applied Science Department, Universiti Teknologi Petronas, 32610 Seri Iskandar, Perak Darul Ridzuan 1Department of Chemistry, Penang Branch, Jalan Tull, 10450 Pulau Pinang

Aflatoxins are a group of secondary metabolites produced by the fungi Aspergillus. The threat from aflatoxins

contamination is especially serious in the tropics and sub-tropics where high temperature and humidity are ideal

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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for the production of molds. The complexity of samples and the low levels of aflatoxins poses considerable chal-

lenge in the analytical determinations prior to their determination. In this presentation, two major strategies to

meet these challenges will be discussed, i.e., (i) Enhancements of analytical signals using post-column photo-

chemical derivatization, and (ii) new sample preparation based on in-syringe- dispersive-micro-solid phase ex-

traction. Green features in these approaches will be highlighted. The analysis of aflatoxins B1, B2, G1, G2 and

M1 in different food matrices such as peanuts, rice and milk will be showcased.

--oOo--

INVITED LECTURE

MOLECULARLY-IMPRINTED POLYMER SOLID-PHASE EXTRACTION FOR

DETERMINATION OF ATRAZINE IN SOIL SAMPLES

Marinah Mohd Ariffin* and Nurul Ashikin Binti Mohyidin

School of Marine and Environmental Sciences, Universiti Malaysia Terengganu, Malaysia

Atrazine is an herbicide used as weeds control and it is harmful to environment and human health. The detection

of atrazine exists in environment always interfered by other matrices when using conventional extraction methods.

Therefore, molecularly imprinted polymer (MIP) for atrazine had been synthesized in order to achieve good re-

producibility and more accurate result. MIP was prepared via bulk polymerization technique with atrazine as a

template. Methacrylic acid (MAA) and ethylene glycol methacrylate acid (EGDMA) were used as monomers and

crosslinker respectively. In order to increase pores size of sorbent, acetonitrile with toluene was used as porogen

and while azobisisobutyronitrile (AIBN) was used as initiator. NIP was prepared following the same methodology

as of with MIP but no addition of template. The polymers were then ground and sieved in the range size of 25 –

38 µm and used as sorbent material for solid phase extraction (SPE). The physical characterizations were done by

using Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) and Brunauer Emmett Teller

(BET). While, the quantitative analysis was conducted by using High Performance Liquid Chromatography and

chromatographic separation using 250 mm x 4.6 mm ID column. Molecularly Imprinted Polymer Solid Phase

Extraction (MISPE) method had been optimized to give higher selectivity and good result. The limit of detection

(LOD) and limit of quantification (LOQ) for atrazine were 0.02 ppm and 0.07 ppm respectively with correlation

coefficient of 0.9997. The recovery values of analytes obtained for MISPE was 64.96% while for Non Imprinted

Solid Phase Extraction (NISPE) was 43.89% respectively. This result shows that MISPE is more selective than

NISPE towards atrazine due to the presence of imprinted sites in MISPE. This research was successfully applied

in soil samples collected at Marang and Manir, Terengganu. From the analysis of soil samples by MISPE and

analyzed by High Performance Liquid Chromatography Ultraviolet Visible (HPLC-UV), concentration of atrazine

detected is below than limit detection. All the samples are free from atrazine contamination.

--oOo--

ELECTROCHEMICAL-INDUCED SYNTHESIS OF NiAl2O4/Al2O3

FOR ADSORPTION OF Pd(II)

Aishah Abdul Jalil1,2

1Centre of Hydrogen Energy, Institute of Future Energy, 2Dept. of Chemical Eng., Fac. of Chemical & Energy Eng.,

Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

A new promising adsorbent, Ni supported on -Al2O3 was prepared in a simple electrolysis system (Ni/Al2O3-E)

in minutes and was compared with the sample prepared by a physical mixing method (Ni/Al2O3-PM). The adsor-

bents were characterized by XRD, TEM, FTIR, 27Al MAS NMR, XPS, and VSM. The results showed that besides

NiO nanoparticles, a NiAl2O4 spinel was also formed in Ni/Al2O3-E during the electrolysis via the dealumination

and isomorphous substitution of Ni2+ ions. In contrast, only agglomerated NiO was found in the Ni/Al2O3-PM.

Adsorption test on removal of Pd2+ ions from aqueous solution showed that the Pd2+ ions were exchanged with

the hydrogen atoms of the surface –OH groups of both adsorbents. Significantly, the Ni/Al2O3-E demonstrated a

higher adsorption towards Pd2+ ions than Ni/Al2O3-PM due to its remarkably higher degree of magnetism, which

came from the NiAl2O4. The use of 0.1 gL−1 Ni/Al2O3-E gave the maximum monolayer adsorption capacity (qm)

of 40.3 mgg−1 at 303 K and pH 5. The Ni/Al2O3-E showed high potential for simultaneous removal of various

noble and transition metal ions and could be also used repetitively without affecting the high adsorptivity for Pd2+

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ions. This work may provide promising adsorbents for recovery of various metals as well as other materials for

such related applications.

--oOo--

SURFACTANT MODIFIED ZEOLITE WITH AMMONIUM, PHOSPHATE AND

POTASSIUM AS REGENERATED CONTROLLED RELEASE FERTILIZER

Norfarah Syuhaidah Mohd Noor, Nik Ahmad Nizam Nik Malek*, Noor Asyraf Noor Azman, M. Arshad Javed

Department of Biotechnology and Medical Engineering, Faculty of Biosciences and Medical Engineering,

Universiti Teknologi Malaysia, 81310 UTM, Skudai, Johor.

The adsorption capabilities of zeolite make it capable to control the release of nutrients for the plant uptake and

improve plant yield. In this study, we managed to load natural zeolite clinoptilolite with major nutrients (N, P and

K) where ammonium and potassium were loaded in the zeolite framework and modification of the zeolite with

surfactant (hexadecyltrimethyl ammonium (HDTMA)) enable it to load with phosphate creating NPK-Organo-

Zeolite. Furthermore, the NPK-Organo-Zeolite could be re-generated forming original zeolite and recycled again

forming NPK-Organo- Zeolite. The performance of re-generated NPK-Organo-Zeolite was studied towards the

growth of Morus alba. Characterization of the studied materials by Fourier transform infrared spectroscopy and

X-ray diffraction found that the HDTMA molecules are attached on the zeolite without distorting the zeolite

framework structure. Two methods of regeneration processes of NPK-Organo-Zeolite were carried out: (1) calci-

nation at 500 ºC of the used NPK-Organo-Zeolite and salt treatment and, (2) heating at 150 ºC and salt treatment.

From the plant growth study against Morus alba, method (2) showed positive effect especially number of leaves,

plant biomass, chlorophyll contents and P content in the leaves. In conclusion, zeolite loaded with N, P and K

could be re-generated and used as recycled repeated controlled release fertilizer.

--oOo--

DISCRIMINATION BETWEEN ARABICA AND ROBUSTA COFFEE BEANS

USING FLAVOR COMPOUNDS

Ku Madihah K.Y.1, Zaibunnisa A.H1 , Osman, R.1 , Misnawi.J.2 , Saim, N.1 * 1Faculty of Applied Sciences, Universiti Teknologi MARA, 40450, Shah Alam, Selangor, Malaysia.

2Indonesia Coffee and Cocoa Research Institute, Jl. PB. Sudirman 90, Jember 60118, Indonesia.

The quality and aroma of roasted coffee are influenced by flavour compounds dominated by pyrizines. In this

study, concentration of pyrazines in roasted Indonesian coffee beans was analysed using headspace solid-phase

microextraction (SPME) coupled with GC-FID. The data obtained from the analysis of 42 samples of Arabica and

Robusta Indonesian coffee beans were subjected to various chemometric methods. Application of principal com-

ponent analysis (PCA) and agglomerative hierarchical clustering (AHC) yielded a clear separation between Ara-

bica and Robusta coffee beans. PCA analysis resulted in two latent factors explaining 76.5% of the total variance.

Discriminant analysis (DA) provided a correct classification of 100% of the coffee beans analyzed. The results

obtained indicated that by applying chemometric methods to data on pyrazines could be useful in the discrimina-

tion of Arabica and Robusta coffee beans.

--oOo--

GREENER, NUTRITIOUS SEED OILS FROM MICROWAVE-ASSISTED

AQUEOUS ENZYMATIC EXTRACTION

Ida Idayu Muhamad1,2*

1Department of Bioprocess & Polymer Engineering, Faculty of Chemical and Energy Engineering 2IJN-UTM Cardiovascular Engineering Centre

Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, MALAYSIA

Microwave assisted aqueous enzymatic extraction (MAAEE) is a promising green technology that is fast, efficient

and energy saving. This method eliminates the disadvantages of conventional solvent extraction method which is

the undesirable effect on oil quality due to the organic solvent usage. Generally, MAAEE process has produced

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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an increment of 10-11% in the oil extraction yield of seeds, revealing the benefits of synergistic microwave enzy-

matic treatment. This mainly due to the hydrolyzed structural polysaccharide of the cell walls and proteins asso-

ciated with the lipid bodies of the seed. The performance and efficiency of MAAEE depend upon several factors

including microwave power, temperature, extraction time, solid to enzyme ratio, and particle size. The physico-

chemical parameters such as density, refractive index, free fatty acid, iodine value, colour, saponification number

and unsaponifiable matter and fatty acids composition of the MAAEE extracted oil were reported quite compara-

ble with those of solvent-extracted oil and control oil, showing no significant (p > 0.05) differences among the

extraction methods. However, the oxidative stability of the MAAEE obtained oil was found to be considerably

improved in comparison to the control oil and solvent-extracted oil as evident by the determinations of conjugated

dienes, conjugated trienes, peroxide and p-anisidine values. It was concluded that microwave-enzymatic adjuvant

improved the oil extraction yield as well as the oxidation properties of the oil produced without altering its other

quality attributes. The present work evaluates and compares the quality characteristics of microwave-assisted

aqueous enzymatic extracted Elateriospermum tapos seed oils with those of hexane-extracted oil and control oil.

Interestingly, MAAEE process has achieved 12% and 16% higher extraction efficiency and concentrated omega-

3 fatty acid respectively compared to non-enzymatic extraction. Although resulted in lower yield than hexane-

extraction (Soxhlet), MAAEE extracted 24% higher concentrated omega-3 fatty acid with almost 99% removal

of amygdalin within 75 second extraction time. Hence the effort to study the interaction of different operating

parameters on the extraction as well as the MAAEE optimization process is sustainably feasible and justifiable.

--oOo--

PROCESSINGS AND CHARACTERISATIONS OF POLYMERIC MATERIALS

FOR SEPARATION PROCESSES

Basuki Wirjosentono*1, Tamrin1, Pevi Riani2, Ridwanto3, Eddyanto4, Ahmad Nasir Pulungan4, Sunit Hendrana5,

Diana Adnanda Nasution1, Hanafi Ismail6, I Putu Mahendra1 1Department of Chemistry, University of Sumatra Utara, Medan 20155, Indonesia

2Polytechnic of Chemical Technology Industry, Medan 20228, Indonesia 3Nusantara Muslim University Al-Washliyah, Medan 20229, Indonesia

4Department of Chemistry, State University of Medan, Deli Serdang 20371, Indonesia 5Physics Research Centre, Indonesian Institute of Sciences, Banten 15314, Indonesia

6School of Materials and Mineral Resources, Universiti Sains Malaysia, Penang Malaysia

* Corresponding author: [email protected]

Various polymeric materials have been processed and characterised and utilized as membranes for separation

processes. Microbentonite-filled polysulphone membranes have been prepared and used for purification especially

on turbidity, pH, total suspended solid (TSS) and total dissolved solid (TDS) of peat water samples. Composition

of the microfiller (200 mesh) was varied from 0-20% (w/w) of total polymer matrix (15% polysulphone in dime-

thyl acetamide solution). It was found that optimum flux of the membrane: 1.31 x 10-5 ml/cm2.s. And after puri-

fication quality parameters of the peat water sample: turbidity: 3.125 NTU, pH 6.8; TSS 52 mg/l and TDS 400

mg/l, which are in accordance with clean water standard according to decree of The Ministry of Health of Indo-

nesia No.416/MENKES/PER/IX/1990. Other work processed natural zeolite of Sarula in North Sumatra Indonesia

to produce nanozeolites after 4 hours continuous heating at 400 oC and ball-milling as filler for chitosan mem-

branes. Optimum water permeation fluxes of the membranes (prepared in 3N acetic acid solution) were obtained:

0.98 – 1.05 kg/m2.hour. Using feeding of 98% ethanol-water mixture at 65 oC, 99.5% of ethanol was obtained in

the separation process. Recently, maleic anhydride-modified deproteinised natural rubber-linkaged to polystyrene

sulphonate membranes were prepared in toluene solution and utilized as polymer electrolyte membrane (PEM)

for hydrogen fuel cell. Deproteinised natural rubber was chosen due to its high elasticity and the polystyrene

sulphonate may function as electrolyte moiety. Characterisation results of the membranes will be reported which

include: FTIR, XRD, SEM, conductivity, water/metanol uptakes, TGA, and mechanical properties.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ROLE OF MOLECULAR MODELLING TO ENHANCE THE UNDERSTANDING

OF SEPARATION SCIENCE STUDY

Hasmerya Maarof

Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor

Separation science studies were commonly associated with experimental and instrumental analysis. With rapid

development in computer technology, various software has been created to aid in understanding a chemical sys-

tem. Moreover, theoretical chemistry has reached a satisfactory level in experiment that allows chemical system

to be simulated in accurate and precise results with minimum resources. Molecular modelling offers a compli-

mentary method by simulating chemical systems; be it small or complex, for better understanding the separation

science study. Examples of problems will be discussed to provide an overview in the role of molecular simulation

such as quantum and molecular mechanics calculations, docking and molecular dynamics that gives researcher a

choice for the best simulation method to use in understanding a system or as a preliminary study in predicting the

outcome of their research.

--oOo--

APPLICATION OF CHIRAL AND NON-CHIRAL HPLC METHOD FOR SELECTED

ANTIFUNGAL DRUG ANALYSIS IN THE PHARMACEUTICAL FORMULATION

Dadan Hermawan1*, Uyi Sulaeman1, Suwandri1, Asmiyenti Djaliasrin Djalil2, Hassan Y. Aboul-Enein3

1Department of Chemistry, Faculty of Mathematics and Natural Sciences,

Universitas Jenderal Soedirman (UNSOED), Purwokerto, Indonesia. 2Faculty of Pharmacy, Universitas Muhammadiyah Purwokerto (UMP), Purwokerto, Indonesia

3Department of Pharmaceutical and and Medicinal Chemistry, Pharmaceutical and Drug Industries Research Division,

National Research Centre (NRC), Dokki, Cairo, Egypt

*Corresponding author: [email protected]

High performance liquid chromatography (HPLC) method using chiral and non-chiral columns has been success-

fully applied in this study for selected antifungal drug (ketoconazole) analysis in the pharmaceutical sample. A

reverse-phase HPLC method using C 8 column was optimized at mobile phase composition containing metha-

nol:water (85:15, v/v) and flow rate of 1.0 mL/min with retention time for ketoconazole less than 3 min. The

average recovery of ketoconazole found in tablet sample was 100.52% (RSD = 0.36%, n = 3). In addition, chiral

separation of two enantiomers of ketoconazole was obtained with resolution (Rs) greater than 1.50 by the HPLC

method using chiral column (Astec cyclobond I 2000 HP-RSP), mobile phase composition containing acetonitrile:

0.1% HCOOH (20:80, v/v) and flow rate of 1.0 mL/min. The present HPLC method was simple, rapid analysis

and less organic solvent used.

--oOo--

ORAL PRESENTATION

MULTI-TRACE METALS FINGERPRINTING OF PENINSULAR MALAYSIA STINGLESS BEE

HONEYS FROM DIFFERENT REGIONS AND SEASONS USING

INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTROMETRY AND

CHEMOMETRIC TECHNIQUES

Syazwani Dzolin1, Wan Aini Wan Ibrahim1, 2* and Naji Arafat Mahat1*

1Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia 2Centre for Sustainable Nanomaterials, Institute of Scientific and Industrial Research,

Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia

*Corresponding author(s): [email protected], [email protected], [email protected]

Consumers’ demand for authenticating and distinguishing the provenance of bee honey is continuously rising.

Considering vast variations in price attributable to different geographical origins, suitable indication on labelling

of honey products remains an important aspect for consumer protection. Since concentrations of trace metals can

be closely related to geographical origin, the use of by spectroscopy and chemometric techniques for ascertaining

the validity of such claim may prove relevant. In this study, eighteen multi-trace metals in stingless bee honey of

Heterotrigona itama species, from different regions and seasons (rainy, max temperature: 27.9°C and less rainy,

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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max temperature: 35.6°C) in Peninsular Malaysia (Kedah, Johor, Selangor and Pahang) were determined by in-

ductively coupled plasma optical emission spectrometry (ICP-OES). Principal component analysis (PCA) was

further applied to recognize the distribution patterns. While the first three principle components for rainy season

(November 2016) accounted for 74% of variance, the same was only 67.6% during the less rainy season (February

2017). Hence, ICP-OES coupled with PCA technique could be used to provide accurate classification of the Ma-

laysian stingless bee honey samples according to their respective origins. This study provided some elemental

information on distribution of stingless bee honey samples at spatial and temporal levels and could be used as a

reference for their provenance establishment and authenticity. Study is in progress to apply linear discriminant

analysis (LDA) to perform further classification. The basic idea of combining PCA and LDA techniques is to

improve the capability for obtaining the best linear classification.

--oOo--

RED MUD AS ALUMINA SOURCE IN THE SYNTHESIS OF MESOPOROUS

ALUMINOSILICATE AND ITS APPLICATION AS CATALYST ESTERIFICATION OF

REUTALIS TRISPERMA OIL

Ahmad Anwarud Dawam*1, Yatim Lailun Ni’mah1, Ratna Ediati1, Didik Prasetyoko1,

Sugeng Triwahyono2, Aishah Abdul Jalil3 1Department of Chemistry, Faculty of Science, Institut Teknologi Sepuluh Nopember (ITS), Surabaya, Indonesia

2Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor, Malaysia 3Dept. of Chemical Eng., Fac. of Chemical and Energy Eng., Universiti Teknologi Malaysia, 81310 UTM Skudai, Johor, Malaysia

Corresponding author: [email protected], Tel: 62-31-5943353 Fax: 62-31-5928314

Red mud is a by-product of the Bayer process and it is composed primarily of fine particles of silica, alumina,

iron, calcium oxide, titanium oxide, and hydroxides. Due to its high calcium and hydroxide content, red mud is

relatively toxic and can pose a serious pollution hazard. In recent years, a great deal of research has been under-

taken to utilize red mud as primary source or secondary source to produce other materials such as basic materials

to produce catalyst or catalyst support, and basic material to produce coal. There are several ways to extract silica

andalumina from red, one of them is alkaline fusion, where alumina and silica reacted with alkaline (NaOH) at

high temperature (550–650 °C). During heating process, sodium aluminate and sodium silicate that soluble in

water will be formed and can be more easily separated. Therefore, red mud can be used as alumina source to

synthesis aluminosilicate material. On the other hand, aluminosilicate materials had various application such as

catalyst, adsorbents, and preparation of siliceous-zeolite membranes. Synthesis of aluminosilicates from commer-

cial chemicals had been widely reported. However, study on the synthesis of amorphous aluminosilicates from

natural raw materials are rarely reported. Red mud was obtained from Bintan Island, Indonesia (Al2O3 28.87 wt%,

SiO2 20,20 wt%). Dried red mud was mixed with NaOH (1:1) in stainless steel crucible. The mixture was then

calcined in furnace at 450°C for 2 hours. Amorphous aluminosilicate (ASM) was prepared by modification of the

method for the synthesis of mesoporous ZSM-5 with a molar compositon of 1 SiO2 : 0.0125 Al2O3 : 0.2 TPAOH

: 38 H2O. In order to produce hydrogen formed ASM, synthesis products were treated with ammonium acetate

solution (0.5 M) at 60°C for 3 h. XRD pattern and FTIR spectra of red mud, fusion product, and amorphous

aluminosilicate indicates iron contents from red mud was successfully separated, and amorphous aluminosilicate

framework was obtained. The N2 adsorption-desorption isotherms of the amorphous aluminosilicates (ASM)

shows a typical pattern of type IV structure with a hysteresis loop (P/P0 = 0,3-1,0) due to the capillary condensation

processes, which is a characteristic of mesoporous material. Pyridine desorption method was used in order to

study acidic properties of amorphous aluminosilicate which identify the presence of Brønsted and Lewis acid sites

(0.012 and 0.215 mmol/g). Morphology and pore appearance of amorphous aluminosilicate studied via SEM and

TEM analysis. It shows that synthesized material consist of unit globular with particle sizes about 100 - 200 nm.

The catalytic activity was studied on the esterification reaction of free fatty acids in Reutealis trisperma (kemiri

sunan) using methanol at temperature 60°C. The conversion of FFA reached up to 37% under the oil to methanol

mol ratio 1:18, 2.5 wt% catalyst, for 2 h of reaction time.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ROBUST AND HIGH THROUGHPUT FIA-MS3 SPECTROMETRY FOR THE

DIFFERENTIATION OF ISOMERIC COMPOUNDS IN DRIED

BLOOD STAIN-APPLICATION TO FORENSIC TOXICOLOGY CASES IN MALAYSIA

Fathiah A. Zubaidi

Department of Chemistry Malaysia, Ministry of Science, Technology and Innovation (MOSTI), 46661, Petaling Jaya, Malaysia.

Prime examples of critical isomeric compound that can co-exist in biological specimen in toxicology cases are

methamphetamine and phentermine. Both compounds have same exact chemical mass and cannot be differenti-

ated by a Mass spectrometer (MS) alone. Street methamphetamine is an illicit substance, while phentermine is a

weight management drug. There are obviously large implications in the misinterpretation of methamphetamine

versus phentermine. Since both compounds are isomeric, even high-resolution mass spectrometry (HRMS) with

accurate mass capability is unable to differentiate these compounds if they are not separable by liquid chromatog-

raphy (LC). However, the MS3 technique can add another dimension in identifying the isomeric compounds by

adding the level of selectivity and using second generation fragments of MRM in MS3 mode. Meanwhile FIA

(Flow Injection Analysis) enables samples to be analysed without column and minimizes run time to 2 minutes

for high throughput analysis. A method was developed for the identification and relative quantitation of isomeric

compounds by using 10ng/mL of methamphetamine and phentermine respectively in dried blood stain (DBS). 20

whole blood specimens which were reported positive for the presence of both drugs were randomly selected and

were individually stained onto the FTA Card. The peaks from the two isomeric compounds were successfully

discriminated for all the 20 tested specimens using the MS3-FIA-MSMS technique. These results suggest that the

technique adds value in identifying and confirming the isomeric compounds of similar masses in the simplest and

rapid analysis.

--oOo--

EFFECT OF CRYSTALLIZATION TIMES ON SYNTHESIS OF ZEOLITE A FROM

VOLCANIC SAND OF KELUD VOLCANO

Sri Setyaningsih, Imroatul Qoniah, Meyga Evi Ferama Sari*, Ratna Ediati1, Didik Prasetyoko1 1Department of Chemistry, Faculty of Science, Institut Teknologi Sepuluh Nopember (ITS), Surabaya, Indonesia

Corresponding author: [email protected] Tel: 62-31-5943353 Fax: 62-31-5928314

Zeolite is a crystalline aluminosilicate material composed of [SiO4]4- and [AlO4]5- tetrahedral which are connected

by oxygen atoms to form cavities and cages. Zeolite has a specific pores and large outside surface so that it can

be utilized as adsorbents, molecular filters and catalysts, ion exchangers and detergent builders. Generally, zeolite

is formed by reaction of aluminum and silica in an alkaline solution. The largest industry of synthetic zeolite is

dominated by detergent industries about 73% of the world's total consumption. The type of zeolite used as a

detergent is zeolite A. In this case, zeolite A is specifically used as ion exchanger. Zeolite formation from com-

mercial materials is too expensive so that the research about zeolite synthesis from natural materials has been

developed to reduce production costs. Zeolite is synthesized from natural materials by two methods, i.e activation

using alkali and hydrothermal method. The activation method using alkali (called as fusion) has been used in

zeolite synthesis to obtain sodium aluminate and sodium silicate derivatives from natural materials. In this study,

zeolite A was synthesized from volcanic sands of Kelud Volcano using two methods, i.e fusion and hydrothermal

process. The product of heating (fusion) process (sodium aluminate and sodium silicate derivatives) is used di-

rectly as reactant without separation. The crystallization time effect on the structural change and the morphology

of zeolite A will be studied. Iron content reduction in volcanic sand of Kelud Volcano was done by Magnetic

Separation and followed by alkali fusion at 550°C for 1.5 h. Zeolite A was prepared with the chemical composition

molar ratios of 0.475 Na2O: 0.047 SiO2: 0.051 Al2O3: 12.8 H2O and crystallization time was varied for 3, 6, 12,

24, 36, and 48 h. XRD pattern of the synthesized sample shows similar pattern. The longer crystallization time

give rise to intensity of characteristics peak zeolite A and particle size of samples. FTIR spectra of samples shows

characteristic band at 466, 551, and 760 cm-1. It also indicates that samples at 36, and 48 h of crystallization time

gives spectra of sodalite while samples at 3, 6, 12, and 24 h gives spectra of zeolite A. SEM images of samples at

different crystallization time proved that longer crystallization time gives transformation from zeolite A to soda-

lite. The crystallization time optimum for zeolite A is 6 hours with crystallinity reaching 43.49%.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ESTERIFICATION OF ACETIC ACID AND BENZYL ALCOHOL OVER ZEOLITE HX

FROM BANGKA BELITUNG KAOLIN

Vita Nur Iftitahiyah1*, Didik Prasetyoko1, Hartati2, Yatim Nailun Nikmah1, Hadi Nur3

1Dept. of Chemistry, Faculty of science, Institut Teknologi Sepuluh Nopember, Kampus ITS Sukolilo, Surabaya 60111, Indonesia 2Dept. of Chemistry, Faculty of science and Technology, Universitas Airlangga, Kampus C, UNAIR, Mulyorejo Surabaya 60115, Indonesia

3Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM, Skudai, Johor, Malaysia

Corresponding Author. E-mail: [email protected] Phone: +62-85-46162520

The esterification of acetic acid (AA) and benzyl alcohol (BA) has been studied over zeolite HX to investigate

activity and selectivity toward benzyl acetate. The detailed optimization of process parameters such as molar

ratio, time of reaction and catalyst loading was also presented. The activity of zeolites are determined by their

intrinsic acidity of both Lewis and Brønsted sites, or by active species (mostly metal ions or oxides) that can be

introduced into the zeolite structure. However, the porosity of zeolite play a crucial role in their shape selectivity.

In particular, HX from faujasite family is composed by sodalit cage and 6-rings (D6R) forming hexagonal and

three-dimensional pore structure that is role in selectivity as catalyst or adsorbent. Zeolite HX is commonly

produced from hydrogels aluminate and sodium silicate, however the synthezised zeolite from alternative source

of silica and alumina such as kaolin continued to be investigated. Kaolin as a alternative source of silica and

alumina are widely available in rocks and minerals. In this research, zeolite HX was syntesized using kaolin

minerals from Bangka Belitung (Sumatra, Indonesia), with the presence of silica (54.9 wt.%), alumina ( 36 wt.%)

and low iron (3.37 wt.%). There were three steps to synthesize zeolite NaX using hydrothermal method; seed

gel, feedstock gel and overall gel, the SiO2/Al2O3 ratio was 4 and the ratio of feedstock gel/seed gel was 18.

Cation exchange of NaX to HX was performed before the catalytic activity test. The synthesized HX powder

was carried out using X-ray Diffraction (XRD), infrared spectroscopy (FTIR), Scanning Electron Microscopy

(SEM), nitrogen adsorption-desorption and pyridine FTIR for acidity. The acidity aimed to determine the amount

of Lewis and Brønsted acid sites of the samples. Surface acidity analysis performed using pyridine adsorption

and analyzed by infrared spectroscopy. The HX has high amount of Lewis (0.1817 mmol/g) and Brønsted (0.053

mmol/g) acid sites. Influence of porous material would be studied on the catalytic activity of the HX in the

esterification reaction. HX was found to be a promising catalyst for benzilation with the higest AA conversion

of 58.78 % was obtained by filtration method and selectivity toward benzyl acetate of 100% was determined by

GCMS. The detailed optimization of process parameters such as molar ratio, time reaction and catalyst loading

over HX were also carried out with aim to maximize AA conversion and also to asses its effect on the catalytic

activity and selectivity. The optimum catalytic condition of molar ratio was 1 : 4. The AA coversion of varying

reaction time and catalyst loading would increase with increasing in reaction time and catalyst loading. The

benzilation mechanism of AA and BA follows Eley-Ridel mechanism.

--oOo--

PREPARATION AND CHARACTERIZATION OF IMPROVED HYDROPHILIC

POLYETHERSULFONE/REDUCED GRAPHENE OXIDE MEMBRANE

Nur Fatihah Tajul Arifin1*, Madzlan Aziz2

1Chemistry Department, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia 2Advanced Membrane Technology Centre, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

Polyethersulfone (PES) has great membrane-forming and excellent physicochemical properties which lead it to

be used widely as a membrane in water treatment. However, PES suffer from fouling due to its’ hydrophobic

characteristics that will affects the performance of the membrane. Thus, reduced graphene oxide (rGO) was cho-

sen in this study to overcome the aforementioned problem. Polyethersulfone (PES)/reduced graphene oxide (rGO)

membrane was prepared by phase inversion method. GO was obtained via modified Hummer’s method and re-

duced to rGO through chemical reduction where NaBH4 was chosen as a reductant. FT-IR was used to study

functional groups left on rGO after reduction process. It showed that the carbonyl and epoxy groups were vanished

after reduction process. Interlayer spacing of GO and rGO were found to be at 7.87 Å and 3.68 Å respectively and

it was obtained by using XRD. The fabricated membrane were characterized using FT-IR to observe any new

bonding formed after addition of GO and rGO. The membrane cross section showed that addition rGO increase

the length of finger-like pores as compared to neat PES when it is observed under SEM. It was observed that the

membrane hydrophilicity enhanced as the contact angle of PES reduced from 69.70O to 32.99O when rGO 24h

was introduced into the polymer matrix. The highest pure water flux obtained was 2904.11 L/m2h. The membranes

showed a lot of enhancement when rGO was used in the polymer matrix.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

16

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ACCELERATED ION-PAIR LC-MS/MS FOR HIGH THROUGHPUT

METABOLITE PROFILING

Zanariah Hashim1*, Tairo Ogura2 and Eiichiro Fukusaki3

1Department of Bioprocess & Polymer Engineering, Faculty of Chemical & Energy Engineering, Universiti Teknologi Malaysia, Malaysia 2Shimadzu Corporation, Kyoto, Japan

3Department of Biotechnology, Graduate School of Engineering, Osaka University, Japan

Ion-pair liquid chromatography/mass spectrometry has been the method of choice for the analysis of intermediates

from central metabolism varying in molecular size and polarity. These intermediates are the key metabolites that

play pivotal role in cellular activities, thus profiling and quantification of them are of prime importance in metab-

olomics studies. For biological samples, often it is desirable to perform analysis in 24-48 h after extraction since

degradation of thermally unstable compounds may occur. In such cases, a fast analysis method is advantageous

especially when dealing with a large number of samples. In this study, a 15 min analysis method employing ion-

pair LC/MS was developed. The LC-MS platform consists of an ultra high performance liquid chromatography

(UHPLC) coupled with a triple quadrupole mass spectrometer (Shimadzu Corp., Kyoto, Japan). Separation was

achieved on a ODS column (150 mm x 2.1 mm, 3 µm) at 40 °C with mobile phase A (97/3 water/methanol with

10 mM tributylamine as an ion pair reagent and 15 mM acetic acid) and B (methanol). The gradient profile is as

follows; 0 min, 0% B; 0.5 min, 0% B; 7.5 min, 25% B; 11 min, 90% B; 11.5 min, 90% B; 11.6 min, 0% B; 15

min, 0% B, with flow rate of 0.3 mL/min. Multiple reaction monitoring (MRM) optimization was performed for

~100 standard metabolites, to determine Q1 and Q3 pre-rod biases and collision energy values. Several types of

stationary phases were tested, and it was found that CERI L-column2 gave the best peak resolution and intensities,

especially for the separation of hexose phosphate isomers, which are typically unresolved in accelerated analysis.

Ultrafast MRM feature enables the detection of numerous compounds in such a short analysis time without com-

promising separation profile. The system was validated using serially diluted standard mixtures and the linear

range and limit of detection were determined. Reproducibility of peak areas was within 20% for most compounds.

The analysis method was further tested using yeast extracts and the system was comparable with previous meth-

ods. This accelerated method is robust enough for routine metabolomics and allows for quantitative analysis with

improved throughput.

--oOo--

DEVELOPMENT OF FTIR DATABASE OF ROSELLE RAW MATERIAL ORIGINATED FROM

WESTERN COASTLINE IN PENINSULAR MALAYSIA

Yew-Keong Choong1*, Nor Syaidatul Akmal Mohd Yousof1, Mohd Isa Wasiman1,

Jamia Azdina Jamal2, Zhari Ismail3 1Phytochemistry Unit, Herbal Medicine Research Centre, Institute for Medical Research, Jalan Pahang, 50588 Kuala Lumpur.

2Drug and Herbal Research, Faculty of Pharmacy, Universiti Kebangsaan Malaysia. 3School of Pharmaceutical Science, Universiti Sains Malaysia.

*Corresponding author: [email protected]; Tel: +603-26162623; Fax: +603-26938210.

The ingredients of Roselle (Hibiscus sabdarifa) have been used as a flavoring agent in the food industry and a

potential herbal medicine in the treatment of hypertension (Wahabi et al., 2010; Hopkins et al., 2013). Herbs from

different geographical regions may differ qualitatively and quantitatively, hence it is crucial to determine the

active components of herbs from different regions and build a reference database. This study focused on the da-

tabase establishment for the authentication of roselle raw material collected at 7 selected locations of western

coastline in Peninsular Malaysia. The calyces of each individual plant were first randomly collected and followed

by washing, drying and grinding. Sample in crude material, was mixed with potassium bromide (KBr) and formed

into a 1mm disk which was scanned 32 times in the range of 4000–400 cm-1 with a resolution of 4 cm-1 using

Fourier Transform Infrared (FTIR) spectrometer. At least 3 discs were produced from each plant calyces and

scanned. The inter-material distance was presented as the mean distance of each sphere created by each batch of

data from different locations. They were clustered with different folder and discriminated by algorithm SIMCA

in the range of 1900 cm-1 to 510cm-1. All the materials from 7 farms achieved 100% separation rate. However, the

only sample that showed 100% (69/69) recognition rate is the roselle from Johor (Muar). This disparity could be

due to the overlapping of similar spectral regions. The average inter material distance of these 7 locations was

9.04. The highest inter material distance was 16.03 among samples from Kedah (Sik) and Selangor (Sabak Ber-

nam), while samples from Perak (Lenggong) and Johor (Batu Pahat) were lowest (4.07). Hence the latter two

locations may be sharing 97.84% similarities of components in roselle grown in similar conditions such as soil,

weather etc. Using FTIR, the geographical origin of an unknown roselle sample can be identified via the estab-

lished roselle spectrum database which can benefit Malaysia Herbal industries for product development.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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IDENTIFICATION OF FLAVONOIDS BIOSYNTHESIS BY AN INDIGENIOUS HERBAL PLANT

FROM BORNEO ISLAND

Khairunnabihah Bachuri, Mariya Tijjani, Anthony Nyangson Steven, Nur Izzati Mohd Noh*

Chemistry Department, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

*Corresponding author : [email protected]

In Borneo Island, a herb called ‘bayur’ is used as a traditional medicine by breast cancer patients. The local people

believe that ‘bayur’ posses anticancer properties. However, there is lack of scientific evidence on the anticancer

activity of the plant. This research is significant in identifying flavonoids because they are bioactive compounds

with antioxidant as well as anti-cancer properties. In this study, a putative Chalcone synthase (CHS) gene, which

encoded for the intermediate enzyme in the biosynthesis pathway of flavonoids, was isolated from an indigenous

unknown plant. Multiple sequence alignment (MSA) results revealed that the putative CHS gene from the indig-

enous unknown plant had 68.2% and 62.7% similarities with CHS gene of Theobroma cacao (database) and T.

cacao (local cocoa variant) respectively. Although the latter has lower similarity compared to the former, these

sequences still share close gene similarities in terms of chemical and physical characteristics (such as positive

residues, hydrophobic residues, polar residues), and identical residual positions in the alignment. They also share

lineage relationship since they were recruited from an ancient primary metabolic system for land adaptation, due

to this the genes evolved structurally and functionally similar. On the other hand, liquid extracts from both leaf

and skin tissues of the indigenous unknown plant were analysed using Liquid Chromatography- Mass Spectrom-

etry to identity the flavonoids synthesized by this plant. The spectrometric analysis resulted in detection of one

chalcone and two flavones. This study proposes a presence of flavonoids metabolic pathway by the indigenous

unknown plant as indicated by both genetic and chemical identification.

--oOo--

MAGNETIC SOLID-PHASE EXTRACTION USING Fe3O4@IONIC

LIQUID-Β-CYCLODEXTRIN POLYMER AS ADSORBENTS FOR ANALYSIS OF AROMATIC

AMINES COUPLED WITH GC-FID

Y. H. Boon1*, M. Raoov1, N. N. M. Zain1, S. Mohamad2, 3 and H. Osman4

1Intergrative Medicine Cluster, Advanced Medical & Dental Institute, Universiti Sains Malaysia, Pulau Pinang 13200, Malaysia 2Department of Chemistry, Faculty of Science,Universiti Malaya, Kuala Lumpur 50603, Malaysia.

3Universiti Malaya Centre for Ionic Liquids (UMCiL), Department of Chemistry, Faculty of Science,

Universiti Malaya, Kuala Lumpur 50603, Malaysia 4School of Chemical Sciences, Universiti Sains Malaysia, Pulau Pinang 11800, Malaysia

In this present work, β-cyclodextrin functionalized ionic liquid polymer (ILs-β-CDCP) was modified with Fe3O4

nanoparticles to prepare magnetic solid phase extraction adsorbents (Fe3O4@ILs-β-CDCP). The properties and

morphology of Fe3O4@ILs-β-CDCP was characterized by Fourier transform infrared spectroscopy (FTIR), Nu-

clear magnetic resonance spectroscopy (NMR) and other characterization instruments. A new method of magnetic

solid phase extraction (MSPE) coupled with gas chromatography-flame ionization detector (GC-FID) for the anal-

ysis of aromatic amines in water samples was established. The influences of several experimental variables (in-

cluding the ionic strength, amount of adsorbents, pH value, extraction and desorption time, sample volume,

strength and volume of desorption solvent, and agitation time) has been considered in depth in the optimization

process to achieve the best extraction efficiency. Analytical calibration equation, detection limit, recovery, and

specificity were determined as well. Fe3O4@ILs-β-CDCP was proved to enhance detection sensitivity with higher

adsorption capacity towards aromatic amines compare to other adsorbents. The results demonstrated that the de-

veloped method is simple, accurate and remarkably free from interference effects.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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PREPARATION OF TERNARY OIL PALM EMPTY FRUIT BUNCH ACTIVATED

CARBON- MAGNETITE-POLYPYRROLE FOR THE EXTRACTION OF ENDOSULFAN

AND DIELDRIN USING RESPONSE SURFACE METHODOLOGY

Faridah Mohd Marsin1,2, Wan Aini Wan Ibrahim1,3*, Hamid Rashidi Nodeh4, Mohd Marsin Sanagi1,3

1 Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310, UTM, Johor Bahru, Johor, Malaysia 2Department of Chemistry (Southern Branch), Jalan Abdul Samad, 80100, Johor Bahru, Johor, Malaysia

3Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research,

Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia 4 School of Chemistry, College of Science, University of Tehran, Tehran, Iran

*Corresponding author [email protected]

The enhancement on oil palm empty fruit bunch - activated carbon-based adsorbent (OPAC) using magnetite and

polypyrrole was studied for the extraction capabilities of two organochlorine pesticides in water, endosulfan and

dieldrin using magnetic solid phase extraction. The effect of three preparation variables, namely magnetite: acti-

vated carbon ratio, amount of polypyrrole monomer, and amount of FeCl3 oxidant on the endosulfan and dieldrin

uptake by the composite was investigated using gas chromatography-micro electron detector (GC-μECD). Based

on the Box-Behnken design, a quadratic model was developed to correlate the three preparation variables to the

response of the two analytes. The adsorbent preparation was optimized using response surface methodology by

maximizing the extraction of two major organochlorine pesticides (endosulfan and dieldrin) in water, within the

ranges studied (R2 < 0.99, p-value < 0.001%). The optimum conditions for preparing the adsorbent with the aim

of affordable and greener extraction method were found to be as follows; magnetite: activated carbon ratio of 2:1

w/w, 1 g of FeCl3 and 100 μL of pyrrole monomer. The experimental results obtained agreed satisfactorily with

the model prediction (> 90% agreement). The surface morphology of the optimized composite showed that the

synthesized magnetite is embedded within the pores of the activated carbon and polypyrrole sealed the activated

carbon to produce an effective ternary adsorbent for the extraction of dieldrin and endosulfan in water matrices.

The functional groups of the synthesized adsorbent were determined from Fourier transform infrared spectros-

copy.

--oOo--

NEW 3-AMINOPROPYLTRIMETHOXYSILANE FUNCTIONALIZED MAGNETIC

SPOROPOLLENIN-BASED GRAPHENE OXIDE ADSORBENT FOR REMOVAL

OF PB(II) FROM AQUEOUS SOLUTION

Abdul-Aziz Mohd Hassan1, 2, Wan Aini Wan Ibrahim1, 3*, Mohd Bakri Bakar1, Mohd Masin Sanagi1,3

1Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia 2Dept. of Pure and Applied Chemistry, Fac. of Science, Kebbi State University of Science and Technology Aliero, Nigeria

3Centre for Sustainable Nanomaterials Ibnu Sina Institute for Scientific and Industrial Research,

Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

Corresponding author; W.A. Wan Ibrahim (UTM), Tel: +60-7-5534311; Fax:+60-7-5566162; email: [email protected]

New 3-Aminopropyltrimethoxysilane functionalized magnetic sporopollenin (MSp@SiO2-NH2-based) graphene

oxide (GO) adsorbent (GO@SiO2-MSp@SiO2-NH2) was successfully synthesized and applied for the first time

in the removal of Pb(II) from aqueous solution. The properties of the composite were characterized using Fourier

transform infrared spectrometry, thermogravimetric analysis, field emission-scanning electron microscopy, en-

ergy dispersive X-Ray analysis, N2 adsorption and vibrating sample magnetometry. Evaluation of the adsorption

performance of GO@SiO2-MSp@SiO2-NH2 at optimum conditions reveals that the adsorbent has a maximum

adsorption capacity of 323 mg/g for Pb(II) at an optimum solution pH of 6.0, 20 mg adsorbent dose and 30 min

contact time at 35oC in 50 – 200 ppm initial Pb(II) concentrations. Initial and final concentrations of Pb2+ in the

water samples were analyzed using atomic absorption spectroscopy. The adsorption behavior of Pb(II) on

GO@SiO2-MSp@SiO2-NH2 was studied using Langmuir and Freundlich isotherms models. The values of coeffi-

cient of determination (R2) showed that the adsorption fitted the Langmuir model. However, kinetics studies sug-

gest that the adsorption followed a pseudo second order rate model and thermodynamic studies reveals that, the

adsorption process is endothermic and spontaneous. The newly synthesized adsorbent can be reused up to seven

times and still retains good adsorption capacity.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ENANTIOMERIC RESOLUTION OF IMIDAZOLE ANTIFUNGAL AGENTS

USING DIFFERENT MODIFIED CYCLODEXTRINS AS CHIRAL SELECTORS IN

CAPILLARY ELECTROPHORESIS.

N. R. Azhari1*, M. Raaov1, N. Yahaya1, F. B. M. Suah2

1Integrative Medicine Cluster, Advanced Medical and Dental Institute (AMDI), Universiti Sains Malaysia, Malaysia. 2School of Chemical Sciences, Universiti Sains Malaysia, Malaysia.

A capillary electrophoresis (CE) method employing a number of native and anionic derivatised cyclodextrins

(CDs) including green ionic liquid-based β-cyclodextrins and 6-O-(sulfo-n-propylether-β-cyclodextrin), were

studied and compared as chiral selectors for the simultaneous enantioseparation of two azole antifungals for the

first time. In this study, five different types of ionic liquids (ILs) and 1,3-propanesultone were employed to syn-

thesize modified β-cyclodextrins. The polymers were characterized using various tools including 1H nuclear mag-

netic resonance spectroscopy (1H-NMR) and Fourier transform infrared spectrophotometer (FTIR) and the result

was compared to native β-cyclodextrin. The CE method was developed and applied to discriminate four stereoi-

somers of ketoconazole and and two stereoisomers miconazole as the subjects of study. The background electro-

lyte (BGE) and chiral selector types, concentrations, pHs, running voltage, capillary temperature, injection types,

and surfactant or additive types, were studied and optimized. Analytical calibration equation, detection limit and

recovery were determined as well. The modified cyclodextrins was proved to enhance the enantioseparation of

ketoconazole and miconazole compared to native β-cyclodextrin not only by changing the electroosmotic flow

and increase solubility of chiral selectors, but also by the hydrophobic interaction, hydrogen bonding, Van Der

Waals, and π-π interactions between the drug molecule and derivatives outside the CDs.

--oOo--

SELECTIVE DETERMINATION OF ACIDIC DRUGS IN WATER SAMPLES

BY ON-LINE SOLID PHASE EXTRACTION LIQUID CHROMATOGRAPHY USING

ALGINATE INCORPORATED MULTI-WALLED CARBON NANOTUBES AS SORBENT

Nurzaimah Zaini @ Othman, Nor Suhaila Mohamad Hanapi, Wan Nazihah Wan Ibrahim and Nor’ashikin Saim

Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

*Corresponding author, E-mail: [email protected] (N.S.M. Hanapi)

Alginate incorporated multiwalled carbon nanotubes sorbent (Ag-MWCNTs) was used as sorbent in online solid

phase extraction liquid chromatography (online SPE-LC) to determine five selected acidic drugs in water samples.

Optimization of online SPE-LC operating parameters such as valve switching time, composition of acetonitrile

and methylsulfonic acid (MSA) and buffer pH was conducted using Box-Behnken Design of Response Surface

Methodology (RSM) to evaluate interactive effect of the variables. Under the optimized conditions (valve switch-

ing time: 1.5 min, composition of acetonitrile:MSA, 60:40 and buffer pH: pH 2), the method gave good linearity

(0.01-100 μg L−1) with coefficient of determination (r2) of 0.9969 - 0.9995 and low limits of detection (0.003 -

0.008 μg L−1). This bioplymer sorbent showed high potential as an alternative sorbent for online SPE-LC with

high degree of selectivity, sensitivity and efficiency.

--oOo--

MICRO-SOLID PHASE EXTRACTION USING ALGINATE/GRAPHENE OXIDE (Alg-GO)

FOR THE DETERMINATION OF SELECTED NON-STEROIDAL

ANTI-INFLAMMATORY DRUGS FROM WATER SAMPLES

Mohammad Salim Tabish, Nor Suhaila Mohamad Hanapi, Nor’ashikin Saim and Wan Nazihah Wan Ibrahim

Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

*Corresponding author, E-mail: [email protected] (N.S.M. Hanapi)

The aim of the present study was to synthesize Alg/GO as newly sorbent for the micro solid phase extraction (µ-

SPE) for the pre-concentration of selected NSAIDs. The resulting material was utilized as sorbent for determina-

tion of three targeted analytes (ibuprofen, naproxen and diclofenac) from water samples prior to high performance

liquid chromatography-diode array detector (HPLC-DAD). The effects of various experimental parameters such

as the percentage composition Alg-GO, extraction time, sample pH, desorption time and stirring speed condi-

tions were optimized. Under the optimum conditions, good linearity was achieved in the 10–500 µg/L with the

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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coefficient of determination (r2) was 0.9992 and low limits of detection (LOD) at 0.2 µg/L. The Alg-GO -µ-

SPE-HPLC-DAD is simple, selective and efficient for the determination of NSAIDs in water samples .

--oOo--

ECO-FRIENDLY MAGNETIC ADSORBENT FOR DISPERSIVE MICRO-SOLID

PHASE EXTRACTION OF NON-STEROIDAL ANTI-INFLAMMATORY

DRUGS FROM AQUEOUS SAMPLES

S. M. Abd. Wahib1*, W. A. Wan Ibrahim1, 2 and M. M. Sanagi1,2

1Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia 2Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research,

Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

Corresponding author: [email protected], [email protected]

As a drive for sustainability, introducing sorbent material with low toxicity, bio-compatible and from renewable

resources is feasible. In the present work, an abundant and low-cost natural polymer namely sporopollenin was

utilized and modified via facile route for use as dispersive-micro-solid phase extraction (D-μ-SPE) adsorbent for

the analysis of four selected non- steroidal anti-inflammatory drugs (NSAIDs) prior to high performance liquid

chromatography. Instead of incorporation with magnetite for rapid separation, sporopollenin was functionalized

with 3-cyanopropyltriethoxysilane (MS-CNPrTEOS) to enhance its extraction capability. Typical magnetite

(Fe3O4) coated with CNPrTEOS (Fe3O4@CNPrTEOS) was prepared as a comparison study. The extraction per-

formance of both materials were evaluated and optimized. Parameters affecting extraction performance were sys-

tematically studied. Results indicated that MS-CNPrTEOS D-μ-SPE exhibited higher extraction performance than

Fe3O4@CNPrTEOS D-μ-SPE, demonstrating the good potential of the former material in extracting the four

NSAIDs in aqueous samples. The viability of the MS-CNPrTEOS D-μ-SPE was assessed using different water

samples and good linearity were obtained with R2 ≥ 0.9951 and good detection limits (LOD = 3 × s'0) were ob-

tained (0.21 - 0.51 µg L-1). The proposed MS-CNPrTEOS D-μ-SPE is simple, fast, cost-effective, eco-friendly

and potentially anticipated for real drugs analysis.

--oOo--

COMPLEX REACTION OF HISTAMINE, METAL AND ALIZARIN RED S AS A NOVEL

SPECTROPHOTOMETRIC METHOD FOR HISTAMINE DETERMINATION IN FISH

Miftakhul Jannatin1*, Ganden Supriyanto1,2

, Pratiwi Pudjiastuti1, Wan Aini Wan Ibrahim3

1Department of Chemistry, Faculty of Science and Technology, Airlangga University, 60115, Surabaya, Indonesia 2Laboratory of Sensor and Biosensor, Institute of Tropical Disease, Airlangga University, 60115, Surabaya, Indonesia

3Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

An analytical method for the determination of histamine using metals and alizarin red S (ARS) reagents using

UV-Vis spectrophotometry was developed. Cu(II) and Co(II) and alizarin red S were usedto form colored complex

with histamine. The developed method was used to detect qualitatively and quantitatively the presence of

histamine. Absorbance of Cu(II) and Co(II) complex were measured at a maximum wavelength of 505.5 and 567

nm respectively. Optimization of analytical parameters such as concentration of metals, concentration of alizarin

red S, sample solution pH, and optimum time were performed. Experimental results showed that the optimum

concentration of Cu(II) was 50 ppm, 75 ppm alizarin red S, sample solution pH 6, and 15 min optimum time,

while the optimum concentration of Co(II) was 125 ppm, alizarin red S was 75 and 50 ppm, sample solution pH

5 and 10 min optimum time. Method validation indicated that the coefficient of variation, limit of detection (LOD)

(S/N =3), and limit of quantitation (LOQ = 10S/N) of Cu(II) were 0.65%, 8.94 ppm, and 29.82 ppm respectively

with a sensitivity of 0.0054/ppm and linearity of 0.9959. Accuracy of histamine determination through Cu-ARS-

histamine complex at a concentration of 50, 100, and 150 ppm were 105.7% (RSD = 0.777%, n = 3), 105.06%

(RSD = 0.606%, n = 3), and 94.12% (RSD = 0.767%, n = 3, respectively. Meanwhile, the coefficient of variation,

LOD, and LOQ of Co(II) were 0.28%; 2.58 ppm; and 8.6 ppm respectively with a sensitivity of 0.0006/ppm and

linearity of 0.9965. Accuracy of histamine determination through Co-ARS-histamine complex at a concentration

of 50, 75, and 125 ppm were 98.33%, 95.83%, 93.88%, respectively. The proposed method was successfully

applied to the determination of histamine in a fish sample with quantitative recovery; for Cu(II) complex (99.23%)

and Co(II) complex (102.62%).

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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POSTER PRESENTATION

PHYSICO-CHEMICAL AND FUNCTIONAL PROPERTIES OF RICE BRAN PROTEIN

HYDROLYZED AND THEIR APPLICATION IN FOOD MODEL.

C. Ratchanee1*, S. Naphapob1, T. Parinya1 and P. Atikorn2

1Department of Innovation and Product Development Technology, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok (Prachinburi campus), Prachinburi, Thailand 2Food Biotechnology Research Unit, National Center for Genetic Engineering and Biotechnology

Thailand Science Park, Khlong Luang, Pathum Thani, Thailand.

Rice bran contains several beneficial compounds, for example, essential amino acids, vitamins and minerals. Be-

sides amino acids, rice bran also contains several vitamins and minerals. Therefore, rice bran and rice bran proteins

could be potentially used in several food applications, for example, functional protein beverages, with low aller-

genic properties. To increase the value of rice bran and extend its application, this research aimed to investigate

some physico-chemical and functional properties of hydrolyzed rice bran protein by enzymatic extracts for poten-

tial use in food model. Enzymatic processes for protein extraction of defatted Kaow Dok mali 105’s rice bran

were produced under condition; enzyme concentration (0.075 gram / 5 gram of protein), extraction temperature

(50C) and extraction time (4 h). The obtained protein solution was further dried using a rotary evaporator and a

freeze dryer, respectively. The hydrolyzed protein powder was analyzed for physical, chemical and functional

properties. Results showed that bulk density and whiteness of rice bran protein (RBP) was 0.450.02 g/ml and

85.551.26, respectively. For moisture (%), protein content (%) and degree of hydrolysis (%) was 7.730.34

22.323.07 and 19.420.72, respectively. The solubility of RBP at pH 4-6 ranged 29.34-42.84%. The functional

properties of RBP followed; the total phenolic content was 7.280.08 mg gallic/ g sample, the antioxidant activi-

ties by DPPH scavenging activity (%) was 4.041.03, FIC (EDTA eq.) was 0.040.007 and ABTS (mg ASC/ g

sample) was 2495.26287.10. The emulsifying properties (EAI) was 8.78 m2/g protein. The foaming capacity (%)

was 35.96-80.19%. Glutamine, Alanine, Valine and Leucine are the major amino acid in RBP. Finally, physical

chemical and microbiological of pasteurized fruit juice (75C 2min. 50sec.) with RBP was evaluated.

--oOo--

KINETIC DEGRADATION OF TOTAL PHENOLIC CONTENT, DPPH RADICLE

SCAVENGING ACTIVITY AND XANTHINE OXIDASE

INHIBITORY ACTIVITY IN YANANG (TILIACORA TRIANDRA) LEAF EXTRACT

S. Eadmusik1*, C. Phungamngoen1 and N. Choosuk2

1Department of Agro-industry Technology and Management, Faculty of Agro-industry,

King Mongkut’s University of Technology North Bangkok, Thailand 2Department of Innovation and Product Development Technology, Faculty of Agro-industry,

King Mongkut’s University of Technology North Bangkok, Thailand

Yanang (Tiliacora triandra (Colebr.) Diels) leaves are usually extracted with water to be cooked with bamboo

shoots because of its xanthine oxidase inhibitory activity. Xanthine oxidase converts hypoxanthine into xanthine

and sequently into uric acid which can accumulate in human body and cause Gout (Gouty Arthritis). Presently,

Canned bamboo shoots in Yanang leaf extract is produced in order to expand shelf-life of bamboo shoots and ease

to prepare food. The objectives of this research were to investigate the effect of different thermal processing during

Yanang leaf extract preparation on total phenolic content, DPPH radicle scavenging activity and xanthine oxidase

inhibitory activity and to determine kinetics of Yanang leaf extract’s quality alterations. The Yanang leaf extract

preparation included 1:12 (w/v) leaves to water ratio, 32,000 rpm blending speed and different heating temperature

at 60, 70 or 80oC for 15 minutes. In order to determine kinetic degradation, data were collected at 0, 1, 3, 6, 9, 12

and 15 minutes of heating time. The results showed that fresh Yanang leaf extract (control sample) had total

phenolic content at 680.16+19.57 mg GAE/100 mg dry weight and it possessed DPPH radicle scavenging and

xanthine oxidase inhibitory activities at 163.53+0.87 µg BHT/mL and 78.58+0.17 %, respectively. The results

also revealed that an increase in heating temperature and heating time decreased total phenolic content and the

activities of Yanang leaf extract. After 15 minutes heating, the total phenolic content of Yanang leaf extract ranged

from 526.33+28.79 to 638.93+29.69 mg GAE/100 mg dry weight, DPPH radicle scavenging activity ranged from

92.86+1.66 to 136.41+5.70 µg BHT/mL and xanthine oxidase inhibitory activity ranged from 72.64+0.34 to

76.65+0.50 %. The change of total phenolic content (R2 = 0.809-0.959) was the zero-order kinetic model and that

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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of DPPH radicle scavenging activity (R2 = 0.783-0.920) and xanthine oxidase inhibitory activity (R2 = 0.864-

0.922) were the second-order.

--oOo--

EFFECT OF PRE-TREATMENT ON THE QUALITY OF DRIED COCONUT

DURING STORAGE

Natthaya Choosuk1, Nattakan Jakkranuhwat1*, Chanthima Phungamngoen2, Patcharee Kunchansombat 2

1Department of Innovation and Product Development Technology, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok, Thailand

2Department of Food Science and Management, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok, Thailand

This study aimed to investigate the effect of pre-treatment conditions on the quality of extended dried coconut for

acceptable to consumer. The research was divided into two experiments. In the first experiment, the two-layer

flesh 8 month-old aromatic coconut (Cocos nucifera L.) after pollination were soaked in sucrose solution

(5%(w/v)) before blanched at 80±2 oC for 2 min, soaked in Potassium metabisulfite: K2S2O5 (0.01, 0.02 and 0.03%

(w/v)) for 5 min and then dried at 60±2°C for 20 h. The color, moisture content (MC), water activity (aw) and

texture of dried coconut were investigated. The second experiment, the qualities of dried coconut obtained from

the first experiment with optimum K2S2O5 concentration were determined during storage in aluminium foil

pouches at 30±1 oC for 91 days. The results from the first experiment showed that the interaction between blanch-

ing and K2S2O5 soaking significantly (P<0.05) affected the color, MC and aw of dried coconut. The blanching (2

min) combination with 0.02% (w/v) K2S2O5 had preserving the best quality of dried coconut with the highest

lightness (L*) and lowest chroma (C*). Dried blanched coconuts combined with K2S2O5 soaking had higher MC

and lower aw than control sample (dried coconut without blanching and K2S2O5 soaking). In the final step, the

results also showed that increase in storage time decreased total SO2, L* values and crispness but increased the

peroxide value and C* values of dried coconut compared to control sample. The sensory evaluation results indi-

cated that, the consumer acceptance was no significantly different between 70-day storage dried coconut and 0-

day storage.

--oOo--

OPTIMIZATION OF HERBAL HEALTH TEA FLAVORED WITH ROASTED RICE GERM

(KHAO DAWK MALI 105) USING RESPONSE SURFACE METHODOLOGY

S. Tipkanon1*, R. Charoen1, W. Savedboworn2 and W. Riansa-ngawong2

1Department of Innovation and Product Development Technology, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok, Thailand. 2Department of Agro-industry Technology and management, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok, Thailand.

Herbs have been used for centuries treat a variety of medical illnesses. They are usually consumed in form of tea,

i.e. an infusion of dried plant part (leaves, flowers, seeds, roots, and bark) steeped in boiling water. Herbal teas

are widely sold in health food store. Available as pure or blended samples, herbal teas are popular because of their

fragrance, antioxidant properties and therapeutic application. Rice germ is a by-product of the rice milling process

which is included in rice bran. Rice germ provides as rich source of protein, fat, dietary fiber and nutrient essential

for life such as phenolic compound, vitamin E, and gamma-amino-butyric acid, etc. which are useful for people.

Thus, the objective of this study was to optimize herbal tea flavored with roasted rice germ (Khao Dawk Mali

105) as a new choice of herbal health tea for consumer. Herbal health tea flavored with roasted rice germ was

formulated by using mixture design and response surface methodology (RSM). The range of three components

were 20-50% dried bael fruit powder (Aegle marmelos (L.) Correa), 20-50% dried pandan (Pandanus amarylli-

folius) leaf powder and 30-70% roasted rice germ to a total of 100%. The optimal formula of the herbal tea flavored

with roasted rice germ consisted of 45.25% of dried bael fruit powder, 21.68% of dried pandan leaf powder, and

33.07% of roasted rice germ. The product contained 4.22% moisture and 3.18% Total ash. For antioxidant activity,

it was found that brewed herbal health tea had 69.03% DPPH scavenging activity and 75.16 mgGAE/100 ml total

phenolic content. Water activity of the product was 0.374. The aerobic plate count was less than 1×102 CFU/g

and yeast and mold were not found. Color with L*, a*, b* values and transmittance of brewed herbal tea were

60.11, -1.43, 14.10, and 75.87%, and it had almost clear greenish-yellow color. Consumer acceptability test using

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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150 consumers indicated that the product was liked very much (Overall liking score = 7.6) and 99.3% of them

accepted the product. If the product is available in the market, 99.3% of them decided to purchase this product.

--oOo--

EFFECT OF PRE-TREATMENTS ON QUALITIES OF MINIMALLY PROCESSED

SHALLOTS (ALLIUM ASCALONICUM L.)

P. Renumarn1*, K.K. Joachim3, C. Phungamngoen2 and N. Choosuk1

1 Department of Innovation and Product Development Technology, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok, Thailand 2 Department of Agro-Industry Technology and Management, Faculty of Agro-Industry,

King Mongkut’s University of Technology North Bangkok, Thailand 3 Food Science -Technology and Economics, University of Applied Sciences Bremerhaven, Germany

The objective of this research was to determine the effects of pre-treatment on the qualities of minimally processed

shallots (Allium ascalonicum L.). The shallot was prepared by blanching in boiled water and cooled down imme-

diately below 20°C by using cool water. After that, the shallots were then peeled and dipped in citric acid pH 4

with 100 ppm of sodium chlorite as acidified sodium chlorite (ASC) solution for 10 min and place into polyeth-

ylene bags as packaging materials. The samples were dipped in tap water as the control. Microbial population

(total bacteria and yeast and mold) and qualities of shallots were evaluated during stored at 5°C. On initial day

storage, ASC treatment was significantly (p<0.05) reduced total bacteria and yeast and mold counts more effective

than control treatment. Moreover, ASC did not affect weight loss and total phenolic content as compared to the

control.

--oOo--

THE USE OF LOW GRADE LIMESTONE IN ACID MINE DRAINAGE TREATMENT

A. Othman1,2*, A. Sulaiman1 and I. Ibrahim2

1Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, Malaysia 2Mineral Research Centre, Department of Mineral and Geoscience Malaysia

Limestone is a versatile material that can be used in many industries such as water treatment, paper making, glass,

food, plastics, paint, rubber, etc. In this study, low grade limestone was used in treating acid mine drainage (AMD).

Limestone with the content of calcium carbonate mineral between 85% to 94% can be classified as low grade

limestone material. AMD can be classified as acidic or pH less than 5, contains high concentration of sulphate

and heavy metals such as arsenic, lead, copper, iron, etc. Low grade limestone was obtained from Pengkalan Hulu,

Perak and AMD sample was obtained from tin tailing pond also from Pengkalan Hulu. Five experiments with

different weights of low grade limestone used were 1, 2, 3, 4 and 5 g, respectively. The different weights of

limestone were added respectively into 1 L beakers that contained 500 mL AMD samples. The AMD samples

with different limestone weights were stirred at 500 rpm by using overhead mechanical stirrer. During the stirring

process, pH values of the solutions were recorded at interval times of 0, 5, 15, 20, 25 and 30 minutes. The AMD

samples with low grade limestone were analysed by using ICP-OES for heavy metals content before and after the

experiments.

--oOo--

FRACTIONATION OF AQUEOUS EXTRACT OF FICUS DELTOIDEA VAR. KUNSTLERI’S

LEAVES USING SOLID PHASE EXTRACTION METHOD FOR ANTICANCER

ACTIVITY ON DU145 CELL LINE

Husnul Hanani Soib1*, Harisun Yaakob1,2,, Mohamad Roji Sarmidi2,3, Mohamad Norisham Mohamad Rosdi1

1Dept. of Bioprocess Engineering, Fac. of Chemical and Energy Engineering, 2Institute of Bioproduct Development 3Innovation Centre in Agritechnology for Advanced Bioprocessing (ICA),

University Teknologi Malaysia, Skudai 81310, Malaysia

Ficus deltoidea var. kunstleri or also known as ‘Mas Cotek’ belongs to the Moraceae family. It is widely used for

postnatal treatment, antidiabetes, anti breast cancer, antinociceptive and antihypertension. In this study, the effects

of flavonoid compounds on anticancer activities of aqueous ethanolic fractions from the leaves of Ficus deltoidea

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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var. kunstleri against prostate cancer cell lines, DU145 were investigated. The aqueous extract of F. deltoidea var.

kunstleri was subjected for fractionation by solid phase extraction method using various concentration of aqueous

- ethanol ranging 20-99.8%. The fractions (fraction I-IV) were screened to obtain the most active fraction through

total phenolic and flavonoid contents and MTT Assay. The induction of apoptosis was evaluated using Annexin

V-FITC/PI while the morphological changes of DU145 cells was assessed using acridine orange/propidium iodide

(AO/PI) staining method. HPLC, FTIR-ATR and LC-MS/MS analysis were conducted for identification and con-

firmation of bioactive compounds. It was found that fraction I which was fractionated using 20% of ethanol ex-

hibited the highest polyphenol contents and highest inhibition against DU145 at 100 g/mL (45.45%). Indeed,

reduction of viability cell by MTT assay using crude extract of Ficus deltoidea var. kunstleri and its active fraction

(I) were also compared. It was revealed that the crude and its active fraction I caused cell reduction by apoptosis

through formation of apoptotic bodies, fragmentation, cell blebbing and cell shrinkage which was confirmed by

AO/PI staining method and Annexin V-FITC/PI. The presence of bioactive compounds of vitexin and isovitexin

were identified by HPLC, FTIR-ATR and LC-MS/MS analysis. Positive correlations had established among total

phenolic and flavonoid content and anti prostate cancer activities. Therefore, these results suggested that flavo-

noids content of Ficus deltoidea var. kunstleri and its fraction I could potentially be used as an anti-cancer agent

for prostate cancer.

--oOo--

ECO-FRIENDLY ANALYSIS OF PARABENS IN COSMETICS BY IN-TUBE

SALT-ASSISTED HOMOGENEOUS LIQUID-LIQUID EXTRACTION AND SUBCRITICAL WATER

CHROMATOGRAPHY WITH ULTRAVIOLET DETECTION

H.-K. Shih, C.-W. Lin, J.-F. Jen*

Department of Chemistry, National Chung Hsing University, Taichung, Taiwan

In recent years, the environmental-friendly approach has been the main direction in the development of analytical

techniques to reduce the organic solvent consumption, extraction time and expense. Sample preparations and

chromatographic processes were considered to have most potential to be greener due to their applying quantity of

organic solvents and thus producing waste solvents. Therefore, efforts to decrease organic solvents used in sample

preparations and in chromatographic processes, time-consuming and laborious nature are always in progress.

Parabens are the most widely used preservatives in cosmetics and personal care products, especially methyl and

propyl paraben are the most common of these. There has been much research on parabens due to their widely

being used. Recently studies have found that parabens having relationship with breast cancer because they ap-

peared amongst breast cancer tumor cells, and the possibility of potentially inducing human breast tumors has

been discussed. In order to protect the cosmetics consumer’s health and safety, the Council Directive 76/768/EC

of the European Community restricts parabens below 0.4% (w / w) for a single type paraben and 0.8% (w / w) for

the total content of parabens in cosmetic products. Therefore, it is important to develop an analytical method to

monitor concentrations of parabens in cosmetic products. An eco-friendly analytical protocol for the determina-

tion of parabens in cosmetics by using in-tube salt-assisted homogeneous liquid liquid extraction (SHLLE) and

subcritical water chromatography (SBWC) was developed. Conditions for the SHLLE and SBWC were examined

and optimized after compromising both techniques. Under the selected conditions, parabens in 5 mL diluted aque-

ous sample solution (at pH 6) were extracted by 200 μL isopropanol through stir-mixing and salting-out by adding

4 g of ammonium sulfate in a home-made glass extraction device. After centrifugation at 3200 rpm for 1 min, the

extractant was collected, dried by nitrogen purging, and re-dissolved in 10 μL water (at pH 10.5) for SBWC with

UV detection. The best performance of the SBWC for parabens was using a polymeric PLRP-S column eluting

with water (pH 10.5 adjusted by phosphate buffer) in a 100oC oven after preheating at 80oC. Under these condi-

tions, detections were linear ranged in 0.75-75 μg/L for methyl paraben and ethyl paraben, and 1.5-150 μg/L for

propyl paraben with regression coefficients in 0.9986 - 0.9993. Detection limits were achieved at the level of

0.07~0.1 μg/L. Recoveries were ranged in 92.3% to 109.6% with relative standard deviations (RSDs) less than

9.2%. The enrichment factors for parabens in the SHLLE process were 238 – 309. In the proposed method only

200 μL isopropanol was used in the whole analytical processes which meet the eco-friendly trend in chemical

analysis. It depicted the proposed method is a simple, inexpensive and environmental-friendly approach for the

analysis of parabens in cosmetic products.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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OPTIMIZATION OF THE PREPARATION OF TERNARY MAGNETITE-GRAPHENE

OXIDE-POLYPYRROLE NANOCOMPOSITE FOR THE EXTRACTION OF

IMIDACLOPRID USING RESPONSE SURFACE METHODOLOGY

Faridah Mohd Marsin1,2, Wan Aini Wan Ibrahim1,3*, Hamid Rashidi Nodeh4, Mohd Marsin Sanagi1,3

1 Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310, UTM, Johor Bahru, Johor, Malaysia 2Department of Chemistry (Southern Branch), Jalan Abdul Samad, 80100, Johor Bahru, Johor, Malaysia

3Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310

UTM Johor Bahru, Johor, Malaysia 4School of Chemistry, College of Science, University of Tehran, Tehran, Iran

*Corresponding author: [email protected]

Imidacloprid is the most commonly used systemic insecticide in the neonicotinoids chemical class category and

has high affinity for water. There seems to be a lack of methodology to determine imidacloprid at low levels due

to its polarity. In this work, a ternary magnetite-graphene oxide-polypyrrole nanocomposite tailored to the extrac-

tion of imidacloprid was prepared with the aid of response surface methodology. Box-Behnken Design was used

to develop a quadratic model to correlate selected preparation variables with the response. The adsorbent prepa-

ration was optimized in order to obtain the most suitable adsorbent for efficient extraction of imidacloprid from

water prior to high-performance liquid chromatography with ultraviolet detection (HPLC-UV). The optimum con-

ditions for preparing the adsorbent were as follows: 5 mL ammonia, 7.5 g FeCl3 oxidant amount, and 0.7 mL

pyrrole monomer. The experimental results obtained were in good agreement (97%) with the model predictions.

The surface morphology of the optimized ternary nanocomposite showed that the synthesized magnetite was in-

corporated within the sheets of the graphene oxide and polypyrrole was sealed by the magnetite to produce an

effective adsorbent for the extraction of imidacloprid in water matrices. The functional groups and magnetization

strength of the synthesized adsorbent were determined using Fourier transform infrared spectroscopy and vibrat-

ing sample magnetometer analysis. This study has proved the potential application of the adsorbent for the extrac-

tion of neonicotinoids from water matrices towards the development of a rapid and green extraction method.

--oOo--

ZIRCONIUM LOADED MESOSTRUCTURED SILICA NANOPARTICLES ADSORBENT FOR

REMOVAL OF HEXAVALENT CHROMIUM FROM AQUEOUS SOLUTION

S. Triwahyonoa*, A.A. Jalilb,c and N. Salamuna

aDept. of Chemistry, Fac. of Science, cDepartment of Chemical Engineering, Faculty of Chemical and Energy Engineering, d Centre of Hydrogen Energy, Institute of Future Energy, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

A one pot method for the preparation of zirconium-loaded mesostructured silica nanoparticles (Zr/MSN) was

developed for the removal of hexavalent chromium (Cr(VI)) from aqueous solutions. XRD, TEM, and BET results

revealed that both MSN and Zr/MSN showed a characteristic highly ordered hexagonal pore structure with a high

BET specific area of 821-1219 m2 g-1. FTIR analysis showed that the presence of Zr diminished the absorbance

band that was assigned to silanol groups of the structural defect sites, while XPS analysis of the binding energy

of Si-O-Zr indicated interactions between the silanol groups and zirconium. The interaction of zirconium and

silanol groups from the structural defect sites generated bidentate zirconium, which acted as an active site for the

adsorption. The experimental results showed that the modification of MSN with zirconium significantly enhanced

the adsorption capacity for Cr(VI). The equilibrium isotherm data showed that the adsorption process was best

described by the Langmuir isotherm with maximum adsorption capacity, 104 mg g-1. The kinetics of Cr(VI) ad-

sorption were described by a pseudo-second-order kinetic model. The thermodynamic properties confirmed that

the adsorption of Cr(VI) onto Zr/MSN was spontaneous and endothermic in nature, while the activation energy

(Ea = 24 kJ mol-1) showed that the adsorption was a chemisorption process.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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ANALYSIS OF STRUCTURE-ACTIVITY RELATIONSHIPS OF CO2 METHANATION

REACTION OVER CARIA BASED CATALYSTS

Susilawati Toemena*, Wan Azelee Wan Abu Bakara, Salmiah Jamal Mat Rosida and Wan Nur Aini Wan Mokhtar

aDepartment of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia. bSchool of Chemical Sciences and Food Technology, Fac. of Science and Tech., Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor

*Corresponding Authors’ E-mail: [email protected]

Ceria based catalyst impregnated with Ru/Mn/Al2O3 was developed in order to to convert the CO2 gas into CH4

gas. Among catalysts used in methanation reaction, Ce was acknowledged with its highly basic and unique redox

properties. From the experimental results, the optimum conditions over potential Ru/Mn/Ce (5:30:65)/Al2O3 cat-

alyst was achieved with 65 wt% of Ce based loading calcined at 1000oC gave 97.73% of CO2 conversion with

formation 91.31% of CH4 at 200oC of reaction temperature. 10 g of the potential catalyst was pre-reduced at 300oC

for 30 minutes in the presence of H2 gas prior to the start of catalytic testing. From the characterization of spent

catalyst, the factor for the catalyst deactivation in this reaction was the particle agglomeration due to the loss of

RuO2 and Mn2O3 species.

--oOo--

IDENTIFICATION OF ANTI-CANCER AGENTS IN AN INDIGENOUS PLANT

USING UHPLC-MS/MS

Khairunnabihah Bachuri1, Nur Izzati Mohd Noh2, Anthony Nyangson Steven1*

1Department of Chemistry, Faculty of Science, Universiti Tekologi Malaysia 2Department of Biosciences & Health Sciences, Faculty of Bioscience & Medical Engineering, Universiti Teknologi Malaysia

*Corresponding author: [email protected]

An indigenous plant from Borneo is used to treat cancer by the indigenous community in Sarawak traditionally.

To support the claim of this plant medicine, screening and identifying of the potential anti-cancer agents of the

plant were done using UHPLC-MS/MS which are Q-TOF MS and Triple, Quad MS. Two methods were used,

extraction using ultra-pure water and decoctions using ethanol. Eight known anti-cancer agent found were Cytar-

abine, Xestoaminol C, Encelin, Burseran, SP 600125, Phytosphingosine, Enigmol and Spisulosine whereas five

potential anti-cancers found are Quinic Acid, Elaidamide, Dihydroceramide C2 and Hetisine. The range concen-

trations of known and potential anti-cancer compounds found were from 0.031-11.73 g/g. Most of the class

compounds found are from sphingolipids, terpernoids and alkaloids. This study successfully served as proof that

the indigenous plant has anti-cancer active compounds and can be further study as potential cure for cancer.

--oOo--

QUANTIFICATION OF FLAVONOIDS FROM LEAVES OF MORINGA OLEIFERA LAM

Norazah Basar, Nurshahira Mohd Rozi

Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, Malaysia

*Corresponding author: [email protected]

Moringa oleifera Lam. (M. oleifera) which is also called “pokok kelor” is known to be a rich source of flavonoids.

Different extraction methods of ethanolic extract including cold maceration, soxhlet, ultrasound-assisted by water

bath and ultrasound-assisted by probe and solid phase extraction were carried out. The extracts were subjected to

qualitative and quantitative analysis to determine the phytochemicals present in the leaf. Qualitative analysis on

the extracts showed that M. oleifera contains flavonoid, tannin, alkaloid, phenol, steroid, quinone and coumarin.

The extracts were further analysed using a reversed phase high performance liquid chromatography to quantify

the contents of isoquercetin, quercetin and kaempferol. Quantification of isoquercetin, quercetin and kaempferol

were found higher using solid phase extraction with 7.98%, 0.86% and 1.11% in w/w%, respectively. The vali-

dated HPLC method was effective and practical for quantification of isoquercetin, quercetin and kaempferol in

M. oleifera leaf extracts.

--oOo--

Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia

Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

27

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VNK SUPPLY & SERVICES Email: [email protected]

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Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia

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[email protected] http://www.utm.my/MySSC/