program & abstract book - utm.my . assalamualaikum and salam sejahtera . i am pleased to welcome...
TRANSCRIPT
PROGRAM & ABSTRACTBOOK
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
1
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
2
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
3
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.
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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
11
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.
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Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia
Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia
12
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
13
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
14
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%.
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Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia
Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia
15
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
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
17
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.
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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.
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Malaysia Separation Science Conference 2017 23-25 Oct 2017, Pulai Springs Resort, Johor, Malaysia
Department of Chemistry, Faculty of Science Universiti Teknologi Malaysia
18
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
19
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
20
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
22
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
23
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
24
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
25
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
26
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
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