brochure general mass spectrometer c146e206

7/27/2019 Brochure General Mass Spectrometer C146E206

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C146-E20

Shimadzus Solutions Provided by Mass Spectrometer

Mass SpectrometerGeneral Product Catalog


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LCMS-8030 LCMS-2020 LCMS-IT-TOF GCMS-QP2010 UltraGCMS-QP2010 SE

GCMS-TQ8030LCMS-8080

NEW

NEWNEW

LCMS-8040

Providing Excellence in Data Quality and Faster Speed, Shimadzu's Unique

Technologies Achieve a New Global Standard in Mass Spectrometry

Shimadzu Corporation, a leader in the development of advanced technologies, introduces three new triple

quadrupole mass spectrometers: LCMS-8040, LCMS-8080 and GCMS-TQ8030. The LCMS-8040 and LCMS-8080

expand the analytical range of Shimadzu's LC-MS/MS lineup while the GCMS-TQ8030 achieves the next pro-

gression in Shimadzus GC-MS history of innovation.

These are new addition to Ultra Fast Mass Spectrometry (UFMS) series, with further enhanced Shimadzu s pro-

prietary high-speed Ultra Fast Technologies.

The UFMS series not only provides higher sensitivity performance but also greater excellence in data quality,

enabling dramatic improvements in analytical throughput and expanding the potential range of applications.

Utilizing the same user-friendly interface as HPLC/UHPLC and GC/GCMS modules, LabSolutions workstation

software provides intuitive functionality for more efficient data processing and an easier, more productive

analytical workflow.

Shimadzu's UFMS Series


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Gas Chromatograph Mass Spectrometer

High throughput Liquid Chromatograph Mass Spectrometer

LCMS-8080

GCMS-TQ8030


LCMS-8040

MRM chromatogram of verapamil (0.5pg/mL) and lodocaine,carbamazepine and cllostazol (5pg/mL)

Comparison of simultaneous analysis results ofthree pesticide compounds by LCMS-8030 and LCMS-8040

LCMS-8080 triple quadrupole LC/MS/MS system that provides both best-in-class sensitivity and excel-

lent quantitation performance. This excellent sensitivity is attained regardless of the situation, whether

in drug development and manufacturing, clinical research, foodstuff and environmental analysis, or

drug screening and excellent control and analysis software realizes a stress-free analysis environment.

The LCMS-8040 is ultra fast and high sensitive triple quadrupole LC/MS/MS system,

which is added on higher sensitivity performance to ultra fast performance of LC-

MS-8030. Improvement of sensitivity for ultra fast MRM and scan mode expands the

potential range of LC/MS/MS applications.

Ultra Fast GC/MS/MS, GCMS-TQ8030, provides ease-of-use of GCMS and analysis ac-

curacy of triple quadrupole mass spectrometer. Ultra fast scan/MRM simultaneous

measurement, which is cultured by LCMS-8030, supports multi component simultane-

ous analysis for small amounts of molecules.

00.00 0.25 0.50 min

20

40

60

80 Verapamil 0 .5 pg/mL

m/z 455.50 > 165.10

S/N 16

1.00

100

200

300

1.25 1.50 min

Lidocaine m/z235.10 > 86.20

Carbamazepine m/z237.10 > 194.00

Cilostazol m/z370.10 > 288.00

5 pg/L

Intensity

Intensity

10 ppb : Cloquintocet-mexyl9.5X 10 ppb : Pyrazosulfuron-ethyl7.4X 10 ppb : Linuron5.2X

8030

ESI+ 336.20 >238.00 415.20 >182.10 246.90 >160.00ESI+

8040

8030

8040

8030

8040

100,000 100 1,000

1.50

1.25

1.00

0.75

0.50

0.25

0.00

1.25

1.00

0.75

0.50

1.50

1.00

0.50

0.00

0.25

0.00

18.0 19.0 min 5.5 6 .0 6.5 7.0 min 14.0 14.5 15.0 min

ESI

Black: Total ion chromatogram(m/z: 45 to 600)

Blue: 275 > 241Red: 275 > 111


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Mass Spectrometer Lineup

LCMS-IT-TOF systems are hybrid high performance liquid chromatograph mass spectrom-

eter systems that include an integrated ion trap (IT) mass spectrometer and time-of-flight

(TOF) mass spectrometer. Therefore, they provide both the MS n capability of IT, plus the

high-resolution and high-accuracy mass analysis capability of TOF.


The LCMS-8030 is a next-generation ultra fast LC/MS/MS system applying to wide range

of liquid chromatograph separation from HPLC to UHPLC systems. Ultrafast positive-neg-

ative ion switching and ultrafast scan speeds maximize analysis throughput.


LCMS-8030

LCMS-IT-TOF

The LCMS-2020 is a ultra fast liquid

chromatograph mass spectrometer

designed for ease of use as an HPLC

detector.

It is a suitable quadrupole mass

spectrometer, which provides high cost

performance, for the routine analysis

work in your laboratory.


LCMS-20202500000

2250000

2000000

1750000

1500000

1250000

1000000

750000

500000

250000

0

0.0 0.5 1.0 1.5 2.0 2.5 min

TIC

212.00

256.00

300.00

344.00

388.00

432.00

476.00

520.00

564.00

608.00

652.00

696.00

740.00

784.00

828.00

Simultaneous MRM Positive-Negative chromatogram of 226 Pesticide Components (10 ng/mL)

Mass Chromatogram of Polyethylene Glycol 400

Mass Spectra of Sildenafil

0.25

Intensity

0

0.5

1.0

1.5

x105

0.5 0.75 1.00 1.25 1.5 1.75 min

Sildenafil C22H30N5O4STheoretical value: 475.2122


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The AXIMA series includes four MALDI-TOF MS models, ranging from a linear-

only model to a system equipped with an ion trap. A key feature of MALDI-TOF

MS systems is their ability to acquire mass spectra directly from solid samples,

such as tissue specimens and microorganisms.

The GCMS-QP2010 Ultra features a newly designed data processing platform that

achieves maximum scan speeds, 20,000 /sec, which is twice as fast as previous

models. It also features an advanced scanning speed protocol (ASSPTM), which is pat-

ented technology that minimizes decrease of sensitivity higher scan speed than

10,000 /sec. ASSPTM realizes higher sensitivity at high scan speed.

Matrix Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometer

Series

Gas Chromatograph Mass Spectrometer

GCMS-QP2010

EI mass spectrum of prednisolone

Mass Spectrum of Bacillus Subtilis

Propyzamide

DiazinonBlack: 1,111 /sec

Red: 5,000 /sec

Blue: 10,000 /sec

Previous method Patented method(ASSP)


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LCMS-2020

LCMS-8080LCMS-8040LCMS-8030

LCMS-IT-TOFAXIMA

Assurance

AXIMAConfidence

AXIMAPerformance

AXIMAResonanceGCMS-QP2010

UltraGCMS-TQ8030

(PSD only)

(Resonance only)

(Resonance only)

Qualificationand

quantitation

Qualificationand

quantitation

Qualificationand

quantitation

Qualificationand

quantitation

Qualificationand

structuralanalysis

Qualification

Qualificationand

structuralanalysis

Application Guide

Mass spectrometers are extremely good at obtaining molecular information, such as molecular weight and structural information. Conse-

quently, they are mainly used for quantitative analysis and structural analysis, but the range of applications is expanding. Since current all

mass spectrometers have many specific characteristics, it is difficult to decide which type of mass spectrometer is optimal for a particular

application based on any simple criteria. This means the system must be selected based on user objectives, such as whether high sensitivity

is required, high resolution is required, or a compact general-purpose system is required.

Representative applications for each type of mass spectrometer are indicated below. Use this chart to help choose the best mass spectrom-

eter for your analytical sample.

Instrument Name

Ionizat ionMethod

Mass

Spectrometer

MS

Main Appl icat ions

EI,CI,NCI

ESI

APCI

APPI

DUIS

MALDI

Quadrupole

Ion Trap

TO F

MS

MS/MS

MS n

NanoESI


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LCMS-2020 GCMS-QP2010Ultra

GCMS-TQ8030LCMS-IT-TOF AXIMA Series

*

LCMS-8080LCMS-8040LCMS-8030

Environmental

Foods

Lifescience/

Pharmaceuticals

Chemis t r y

C l i n i c a lR e s e a r c h

Forensics

Atmosphere

Soil

Water

Ingredient analysis

Additives

Residual Pesticide

Toxins

Genomics

Proteomics

Metabolomics

Synthetic compound

impurities

HTS

Pharmacokinetics

toxicity test

Drug product

low-molecular-weight

organic molecules

Polymer composition analysis

Additives

Impurities

Monitoring pharmaceuticals

Endocrinology research

Toxicology

Biomarker discovery

Doping testing

Identification of target substances

Benzene, trichloroethylene,

tetrachloroethylene,

dichloromethane, etc.

Trichloroethylene,

tetrachloroethylene,

dichloromethane, etc.

Pesticides, PFOS/PFOA,

algae bloom toxin, shellfish toxin, etc.

Amino acids, sugars,

catechins, vitamins, etc.

Colorings, antibacterial agents, etc.

Insecticides, disinfectants,

herbicides, etc.

Mycotoxins, etc.

DNA, RNA

Proteins, peptides

Organic acids,

amino acids, lipids, etc.

Pharmaceutical impurities, etc.

Candidate compounds, etc.

Metabolites, etc.

Candidate compounds, etc.

Residual solvents, etc.

Surfactants, antioxidants,

fullerenes, etc.

Polymers, rubber, plastics, etc.

Plasticizers, etc.

Organic impurities, etc.

Pharmaceuticals for treatment, etc.

Hormones, etc.

Acutely toxic substances, etc.

Organic low-molecular-weight molecules, peptides, etc.

Steroids, etc.

Abused substances, etc.

Low-molecular-weight compounds,

antibiotics, antibacterial agents,

natural medicines, steroids, etc.

* Primary structural analysis, excluding calculations of average molecular weight, degree of polymerization, and degree of dispersion


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Mass spectrometers must first ionize sample molecules.

Many type of ionization have been developed.

Electron ionization (EI) ionizes samples using accelerated thermal electrons,

70 eV. EI is generally used for samples, whose molecular weight is less than

1000. It is typically used in combination with a gas chromatograph to ana-

lyze highly volatile molecules or gases.

Electrospray ionization (ESI) ionizes samples in solution by spraying them. It

is mainly used in combination with liquid chromatographs.

Matrix Assisted Laser Desorption/Ionization (MALDI) desorbs sample mole-

cules by laser energy and ionizes those by transferring charge from matrix

ions. MALDI can apply wide range of samples by changing matrix reagents,

hence, this ionization method apply to synthetic polymer and complicated

samples.

8

ESI (Electrospray Ionization)

A sample solution is introduced to capillary applying high electric

voltage and sprayed at the edge of capillary. Droplets of sample

solutions are charged and sample molecules are ionized in liquid

phase.

ESI is best suited to ionizing medium-to-high polarity substances,

peptides, proteins, and oligonucleotides.

DUIS (ESI+APCI)

The DUIS-2020 is a dual ion source that ionizes samples using both

ESI and APCI (atmospheric pressure chemical ionization) modes.

This is best suited to ionizing low-to-medium polarity substances.

MALDI(Matrix Assisted LaserDesorption/Ionization)

After applying the sample and matrices solution on a sample target

and dry up, laser irradiates to sample spot. The sample and matrix

molecules are desorbed and ionized, rapidly.

MALDI enables to ionize high molecular weight compounds, such

as proteins and polymers without dissociation.

ESI

(1) Capillary

(2) Nebulizer gas

(3) Dry gas

(4) DL (desolvation line)

ESI probe

From column

DUIS

Sample target

Sample

Sample target

ESI probe

(1)

(1)

Vacuum

Laser

(2)

(2) (3) (4)

(3) (4)

From column

(1) Nebulizer gas

(2) Corona needle

(3) Dry gas

(4) DL (desolvation line)

: Sample molecules: Matrix: Positive ions: Negative Ions

Molecular Weight

1000100 5000 10000 100000

Middle Polarity

Low Polarity

High Polarity

MALDI

LCMS

GCMS


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Generated ions are separated and

detected based on differences

in their mass-to-charge ratio (m/z value).

Quadrupole Models

Quadrupole mass spectrometers use a set of four parallel electrode

rods to form an electric field.

This electric field is used to separate ions passing through the space

formed by four rods based on their m/zvalue.

Triple quadrupole mass spectrometers use three sets of quadru-

poles configured in series to quantitatively analyze target molecules

in highly contaminated samples, such as pesticides in foods, with

extremely high sensitivity levels.

Time-of-Fl ight (TOF) Models

The velocity of ions, which is accelerated by a fixed electric voltage,

is depending on their m/zvalue.

The velocity of lower m/z ion becomes faster.

Time-of-flight mass spectrometer calculates m/zvalue from the ion

velocity, i.e., time of flight of each ion, which takes to travel a fixed

distance.

Hybrid ModelsHybrid mass spectrometers are a combination of an ion trap mass

spectrometer and a time-of-flight mass spectrometer.

An ion trap consists of two end cap and one single ring electrodes.

An electric field formed by single ring electrode can trap ions in the

space.

A key feature of ion trap is high sensitive analysis and MSn analysis.

Time-of-flight mass spectrometer can determine m/z values with

high accuracy. Ion Trap Dual Stage Reflectron

Detector

Ion Source Quadrupole Detector

Ion source Detector


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LabSolutions LCMS

Method Optimization

In MRM analysis, setting the MRM parameters, such as the m/z

values for precursor ions (Q1) and product ions (Q3) and collision

energy (CE) voltage, is extremely important.

LabSolutions LCMS sets these parameters automatically.

This optimization process enables analyzing target compounds with

high sensitivity.

The method optimization window is shown to the right.

In addition to optimizing MRM parameters, the function enables

product ion searches as well.

Default settings can generally be used for electric voltage optimiza-

tion and automatic product m/zselection settings, but it is also pos-

sible to change detailed settings, such as the number of selected

product ions and the CE step size.

LabSolutions LCMS software offers high functionality, yet is easy to

operate.

Software LCMS-8030/8040

Parameters optimized forhigh-sensitivity detectionof target components

Easily check optimization resultson the window


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Software LCMS-2020

12

LabSolutions LCMS

Data Browser

Quantitation Browser

The data browser allows detecting peaks, analyzing multiple sets of

data, and comparing chromatograms and spectra, all on a single

screen.

The extensive and intuitive user interface supports the postrun anal-

ysis of the huge amount of data generated.

It also allows displaying MS, PDA, and LC chromatograms tiled side-

by-side or overlaid.

The highly flexible report formatting function allows creating fo-

cused reports tailored to analytical operations, such as chromato-

grams, calibration curves, quantitative results, and summary reports.

The quantitation browser has four views; a [Quantitative Results

View] for displaying the quantitative calculation results for each set

of data, a [Method View] for displaying parameters in method files,

a [Chromatogram View] for displaying chromatograms and sample

information, and a [Calibration Curve/Spectrum View] for displaying

the calibration curves and spectra for compounds.

By editing a single method file, the data processing parameters in

that method can be used to perform quantitative calculations on

multiple sets of data.

Quantitative calculation results for up to 1,024 data files acquired

using the same method file can be collectively checked.

LabSolut

LabSolutions LCMS is workstation software used for LCMS system

control and data processing.

LabSolutions LCMS is operated in the same manner as LCsolution,

GCsolution, and GCMSsolution, which means even an inexperi-

enced operator can do everything from making instrument tuning to

setting analytical conditions, viewing or analyzing data, and prepar-

ing reports easily.

The mass spectrometer can be operated in the same manner as ab-

sorption or fluorescence detectors.


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Open Solution

Open Solution is open access software for LCMS-2020 systems. It

allows using Internet Explorer to confirm analytical results or output

reports from any computer on the network. Open Solution provides

a simple user interface that does not require detailed knowledge

about analytical operations.

Start analyses in only three steps. Simply log into Open Solution

(Step 1), specify the minimum required settings, such as registering

samples and specifying the analytical method, and place the vial in

the specified position (Step 2). Then click the start button (Step 3).

Data can be viewed and analytical instrument status monitored

from a separate office. When an analysis is finished, an email is

automatically sent to pre-registered email addresses. This email

includes a web address for viewing the data, where analyticalresults can be easily confirmed and printed.

Laboratory

Office

Internet Explorer Internet Explorer Internet Explorer

Internet Explorer

Open Solution(Web server)Internet Explorer

LCMSsolution


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Software LCMS-IT-TOF

14

LCMSsolution

Data Acquisition

LCMSsolution not only allows tuning instrument parameters, but it

also enables easily setting mode-specific analytical conditions for a

wide variety of measurement modes.

An assistant bar ensures that even inexperienced users can navigate

settings and operations to perform analyses easily.

Parameters for the Mass Spectrometer can be specified in manual,

auto, or direct event event. Parameters for the liquid chromatograph

can be specified in a simple or detailed mode.

These allow using a wide range of analytical conditions.

Data Processing

Data processing function analyzes the high-throughput and high-ac-

curacy data obtained from the LCMS-IT-TOF system with minimal

stress to the operation and quickly provides the necessary informa-

tion.

The data browser feature allows loading and viewing up to 64 sets

of data at the same time.

Files can be managed using intuitive operations.

The quantitation browser enables simultaneously processing quanti-

tation results from multiple sets of data acquired using the same

method.

A wide selection of identification and quantitative processing func-

tions help to shorten the time for data analysis operations.

LCMSsolution is workstation software used for LCMS-IT-TOF system

control and data processing.

Because it is designed on the basis of sample concept of the work-

stations for other chromatograph products, it can be operated in the

same manner as LC, GC and GCMS. Furthermore, it ensures users

can use its functionality efficiently, such as auto-tuning the entire

system and automatic MS/MS functionality, even on more compli-

cated hybrid MS/MS systems.

s

s

s


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Formula Predictor

Formula Predictor is software used to predict the chemical composi-

tion formula of target peak.

It uses a proprietary method to efficiently narrow down the number

of candidates.

MetID Solution

This software compares data from samples before and after they

are metabolized to search for expected and unknown metabolites.

Protein Analysis Software

This software automates operations ranging from sample analysis

to protein identification.

Profi l ing Solution Ver.1.1

This data viewer enables processing multiple files at the same time.

It can be used to correct retention times and normalize mass

accuracy and signal intensity.

It also allows exporting data for use in commercial multivariate

analysis software.

Open Solution ComponentID

This is open-access software for LCMS-IT-TOF systems.

Because this software can be operated without any special detailed

knowledge, it eliminates the need for a specialized operator and

provides an environment where anyone can perform analyses easily.


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Software GCMS

16

GCMSsolution

GCMS Analysis Program

This is used to specify GCMS system configuration, MS tuning pa-

rameters, analytical conditions, and batch processing parameters for

continuous analyses.

It also displays a window for monitoring the system status, allowing

continuously monitoring the status of both the GC and MS units.

The display of usage count for consumables allows viewing estimat-

ed maintenance periods at a glance.

Flexible Report Creation Function

Report formats can be edited easily by put a given size of desired report elements at a target location and within a blank report window.

A variety of elements are available for including in reports, such as chromatograms, spectral search results, and quantitation results.

GCMSsolution is workstation software for the GCMS-QP2010 series

and GCMS-TQ8030.

It uses One-Window technology to display information in a layout

optimized to accurately and quickly acquire data and perform quali-

tative and quantitative analyses.

Preview Print


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GC/MS Method Package Ver. 2 forResidual Pesticides in Foods

Compound Composer DatabaseSoftware for Simultaneous Analysis

This package contains method files for quantitative analysis of 542

pesticides.

These methods include analytical parameters optimized for residual

pesticides in food. It also attach a glass insert suited to pesticide

analysis and specifies which columns to use, which eliminates any

doubt about setting analytical conditions or selecting parts.

This database includes information registered for 942 environmen-

tal pollutant compounds.

This enables identifying and estimating the concentration of

environmental pollutants, residual pesticides, and other substances

without using standard samples.

MS spectra, retention indexes, CAS number, compound name,

molecular formula of 3,000 flavor and fragrance compounds are

included. By utilizing both MS spectrum and retention index, high

accurate identification results can be provided.

GC/MS Forensic Toxicological Database

This database includes 1,011 mass spectra for 502 components

including their free bases and TMS and TFA derivatives, that are

necessary for forensic analysis, such as drugs of abuse, psychotropic

drugs, general drugs, and pesticides.

For components often linked to poisoning, quantitative values can

be estimated without using standard samples.

Other Libraries

Pesticide Library Ver. 3 for Foods

Mass spectra for 578 pesticides measured using electron ionization (EI) and

383 pesticides measured using negative chemical ionization (NCI).

NIST Library

This library contains 243,893 spectra for 212,961 general compounds.

Wiley Library (9th edition)

This library contains about 662,000 spectra for about 592,000 general

compounds.

Drug Library

This library contains spectra for 7,840 compounds including drugs, toxins,

pesticides, and environmental pollutants.

It includes information on.

VOC Analysis Software

This software includes a library for 74 volatile organic compounds.

GC/MS Metabolite Component Database(amino acids, fatty acids, and organic acids)

Flavor & Fragrance Natural & SyntheticCompounds GCMS library Ver. 2 (FFNSC 2)

n-alkaneanalysis data

Masses,calibrationcurves,spectra

Masses, calibration curves,spectra Predictedretention times(target compounds)

Retention times(target compoundsn-alkane) GCMSsolution

method

Database

Compound Composer

Index

Handbook

This database includes retention indices and mass spectra for 311

metabolites (amino acids, fatty acids, and organic acids).

It also includes method files with optimized sample and data

analysis settings, reducing the effort required for determining

analytical conditions and postrun analyses.The measured spectrum (retention index 1090) andthe spectra of compounds with a high score runninga library search

Measured massspectrum

Candidate 1(Similarity : 95)

Candidate 2(Similarity : 95)

Simple library search results

Result after filtering with the retention index(retention index allowance: 10)

Searching both the MS spectrum andretention index enhances reliability ofidentification.

Compound


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Software AXIMA

18

LAUNCHPADTM

Data Acquisition

This software is intuitive and easy to understand, with features such

as a CCD window for monitoring the laser light irradiation status

and a window that indicates the instrument status.

This makes the MALDI-TOF MS system easy to use, even for first-

time users.

An Autoquality function enables automatically optimizing parame-

ters during measurements to keep the quality of mass spectra data

acquired by automatic measurements.

Data Analysis

The peak processing function can select the several type of settings

window from a drop-down list, ranging from a simple settings

window to a detailed settings window, based on the user experi-

ence level.

Seamless integration with many optional software programs en-

sures smooth data analysis.

Measurement data can be exported in a variety of formats to allow

further analysis using third-party software. Batch processing is also

possible.

Protein identification optional software can perform from MALDI-

MS to MS/MS analysis, Mascot search, automatically.

LAUNCHPADTM is workstation software for controlling and process-

ing data from MALDI-TOF MS (AXIMA series) systems.


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Po lymersSoftware for MicroorganismIdent i f i cat ion System

This software is used to analyze not only homopolymers, but also

complicated copolymer compounds as well.

This software identifies microorganisms based by peak pattern

matching.

This software uses automatically analyze sample fractions spots on

a MALDI sample plate, which are separated by HPLC and loaded by

spotting system (AccuSpot).

MALDI MS Imaging Software

This software is used for MS imaging.

It is especially useful for measuring the distribution of new drugs

and metabolite products on tissue specimens.

Software forAccurate Glycan Analyzer 2LC-MALDI

This software is used to identify the structure of glycans.

Used in combination with an AXIMA Resonance system, it allows

identifying glycan structures with high precision.

4000 6000 8000 10000 12000 14000

7271.93

7707.16

8325.38

7333.07

9064.89

6255.85

9738.82

11183.73

10298.41

5382.30

4365.97

10692.83

13001.25

13803.27

Escherichia coli NBRC 3972%Int.

0

10

20

30

40

50

60

70

80

90

100

6601.17

5257.39

13670.54

5819.04

11144.40

9210.48

4522.16

7429.52

13878.63

11636.03

5464.66

7994.51

10379.52

10007.47

12907.95

m/z

%Int.

0

10

20

30

40

50

60

70

80

90

100

Bacillus subtilis NBRC 3134


20/3420

Systems

GCMS

Headspace Analysis SystemHeadspace analysis systems are used for qualitative and quantita-

tive analysis of substances such as flavorings in foods, odors in

chemical products, volatile organic compounds (VOCs) in public

drinking water, environmental water, or waste water, and residual

solvents in pharmaceuticals.

Purge & Trap Analysis SystemPurge and trap analysis systems are used to perform highly sensi-

tive measurements of VOCs or moldy odor-causing substances in

public drinking water, rivers, groundwater, and so on.

LCMS

LCMS-2020 Preparative System

This high-throughput preparative purification system is made pos-

sible by combining LCMSsolution with an instrument control solu-

tion capable of controlling the Gilson 215 Liquid Handler and IFC

PAL liquid handler from CTC Analytics.

2-Dimensional LC/L CMS-IT-TOF System

Co-Sense impurit ies LCMS-IT-TOF is an LC-MS system with

column-switching technology that is designed specifically for ana-

lyzing impurities.

Existing HPLC methods, such as those using phosphate buffer

solutions or ion pair reagents, are used for the fist dimension to

identify peaks required for structural analysis. A mobile phasesuited to LC-MS is used to separate components in the second

dimension before introduction to the LC-MS system.

Pyrolysis SystemThis system thermally decomposes polymer materials, such as plas-

tics, rubbers and resins, over 500 C and analyzes the resulting

pyrolysates with GC/MS.

It is used for structural analysis of polymer compounds, such as

plastics and rubbers.

Thermal Desorption SystemThis system prepares samples for introduction into a GS-MS system

by using thermal desorption to decompose volatile organic com-

pounds collected in a tube filled with adsorbent material.

Samples can also be placed directly in the tube and heated to ana-

lyze the evolved gases.


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Solid Phase Microextraction (SPME) SystemSolid phase microextraction (SPME) enables the analysis of organic

substances with high sensitivity by first concentrating organic sub-

stances in a water or gas phase onto SPME fibers, then desorbing

the substances in the GC injection unit.

Using an AOC-5000 Plus autosampler enables automating the

entire process and ensuring good reproducibility.

GC GC-MS SystemThis system separates components using two columns with differ-

ent polarity.

Unlike multi-dimensional analysis, this system provides compre-

hensive 2-dimensional separation across the entire chromatogram

by repeatedly injecting samples into the second column in an

extremely short time.

AXIMA

SEC-MALDI (LC-MALDI) System

The SEC-MALDI system first separates samples into their compo-

nents by size exclusion chromatography (SEC), then measures the

components using MALDI-TOF MS. This is especially useful for

analyzing mixtures containing multiple components, such as syn-

thetic polymers.

CHIP-1000/MALDI Imaging System

The CHIP-1000/MALDI imaging system is new technology that

uses MALDI-TOF mass spectrometry to directly measure biological

molecules and metabolites on tissue specimens, without sample

extraction or labeling. The system displays the 2-dimensional

distribution of the targeted biological molecules, based on their

positional information and the signal intensities of detected ions.

Direct Sample Inject ion SystemDirect sample injection is a method of bypassing the gas chromato-

graph (GC) and injecting samples directly into the ion source.

This is especially suited to analyzing non-volatile compounds or ther-

mally unstable compounds, which are difficult to analyze in a GC

unit.

Multifunct ional Sample Inject ion SystemThe OPTIC-4 is a GC injection port that enables using various

GC/MS sample injection modes, such as high volume injection,

injection port derivativization, thermal desorption, or DMI (difficult

matrix introduction).

Used in combination with an AOC-5000 Plus autosampler, inserts

can be replaced automatically to increase productivity during mul-

tianalyte analysis.


22/3422

Applications

LCMS-8040/8030

Biomarker Discovery Using LCMS-IT-TOF

Quantitat ive and Qualitat ive Analysis of Plant Hormone Metabolites

LCMS-IT-TOF

Low-molecular-weight compounds in biological

organisms, such as endogenous metabolites in

blood and tissue, are remarkable as biomarker

candidates. An example of using LCMS-IT-TOF

to discover biomarkers in blood plasma from a

type II diabetes model rat (Zucker rat) is shown

below.

After pretreatment, samples were analyzed

using LCMS- I T-TOF. Then the dif ferences

between the groups of normal and type I I

diabetes model rats were detected by primary

component analysis using multivariate analysis

software.

LC/MS/MS systems are an essential tool for quantitative and

qualitative analysis of bioactive substances, which only exist

in small amounts in organisms. An example of using

LC/MS/MS to analyze metabolites of the plant hormone

indole-3-acetic acid (IAA) is shown. All 7 types of IAA

metabolites can be detected by MRM measurement from 1

nM, which allowed creating a calibration curve from 1 to

1000 nM.

In addition, all seven metabolite types were detected in a

measurement of a rice root sample doped 10 M IAA.

Formula Prediction Example

Metabolite Array

Mass Chromatogram and MS andMS/MS Spectra for Components that Varied

Primary Component Analysis Results

Type II diabetes model rat Normal rat

MRM Chromatogram of Metabolitesin Rice Root Sample Doped 10 M IAA

Concentration of Metabolitesin Rice Root SampleDoped 10 M IAA

0

1.0

2.0

3.0

4.0

1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 min

Area (10,000,000)

1:IAA-Asp2:OxlAA (x60)3:DiOxlAA (x35)4:DiOxIAA-Asp (x4)5:DiOxIAA-Glu (x30)6:ICA-Glc (x130)7:OxlAA-Glc (x3600)

Structural Formula of 7 Types of IAA Metabolites

(291>130, posi ti ve ) (192>146, posi ti ve ) (208>146, posi ti ve ) (323>146, posi ti ve )

IAA-Asp OxIAA DiOxIAA DiOxIAA-Asp

(337>146, positive)

DiOxIAA-Glu

(322>89, negative)

ICA-Glc

(352>190, negative)

OxIAA-Glc

N

H

NH

O

COOH

COOH

N

H

O

COOH

N

H

O

HOCOOH

N

H

NH

O

COOH

COOH

HO

O

NH

NH

O

COOH

COOH

HO

ONH

O

O

HO

HO

O

OH

OH

NH

O

HO

O

O

HO

HO

O

OH

OH

Calibration Curve of ICA-Glc

0

0.5

1.0

0 250 500 750 Conc.

Area(100,000)

MRM Chromatogram of ICA-Glc

MRM Chromatogram of DiOxIAA

Compound

IAA-Asp

OxIAA

DiOxIAA

DiOxIAA-Asp

DiOxIAA-Glu

ICA-Glc

OxIAA-Glc

Conc. (nmol/L)

781

5.31

17.1

156

11.9

16.4

1.60

322/89

(Negative)

208/146(povitive)

Mass chromatogram

MS spectrum MS2 spectrum

Precursor ion

(Type II diabetes model rat)


23/34

AXIMA

Analysis of Amino, Organic, and Fatty Acids Using GC/MS Metabolite Component Database

Identification of Glycan Structures Using the Accurate Glycan Analyzer and AXIMA Resonance

GCMS

GC-MS systems are often used in metabolomic and biochemical diagnostic research fields to measure amino acids, organic acids, or

fatty acids in urine or blood. Shimadzu worked jointly with the Shimane University Faculty of Medicine to develop a GC/MS Metabolite

Component Database, containing information on over 300 types of metabolites and other substances (amino acids, organic acids, and

fatty acids). The figures below show results from using this database to analyze fats and fatty acids in human blood serum and show

results from simultaneous analysis of organic acid, amino acid, saccharide, and other metabolites in canine cerebral fluid, conducted

jointly with Osaka Prefecture University Graduate School of L ife and Environmental Sciences associate professor Shigeo Takenaka.

Since many proteins are modified by glycans, the glycans to which they are bonded can have a significant influence on protein function.

The structure of multiple branched molecules, such as glycans, cannot be determined from simple mass spectra, but using MS n analysis

allows identifying different structures of even glycans with identical masses. In this case, by following software instructions up to MS 3

analysis, the system was able to distinguish between the structures of two types of pyridylamino derivatives of N-glycans with identical

masses (m/z1725) that differed only in the position of glucose bonds on non-reducing terminals.

Total Ion Current Chromatogram (TIC) of TMSs in Canine Cerebral Fluid

Component numbers correspond to serial numbers in the GC/MS Metabolite Component Database.

Total Ion Current Chromatogram (TIC) of Methyl Fatty Acids

in Blood Serum

Mass Spectra MS/MS and MS3 Spectra Search Results Based on MS3 Spectra

0

100

200 400 600 800 1000 1200 1400 1600

m/z

200 400 600 800 1000 1200m/z

128042

1707.62

1280.42

915.29

1077.33712.20

1725.64

915.30

712.21

1077.34

550.14388.08

0

100

300 500 700 900 1100 1300 1500 1700

300 500 700 900 1100 1300m/z

0

100

%Int.

m/z

1280.45

915.301342.49

712.22 1077.32

%Int.

0

20

40

60

80

100%Int.

Fraction 2)1725.63

1725.63

m/z

1 690 1 700 1 710 1 720 1 730 1 740 1 75 0 1 760 1 77 0 1 780

0

20

40

60

80

100%Int.

Fraction 4)

m/z

1690 1700 1710 1720 1730 1740 1750 1760 1770 1780

1570.91

1725.71

1707.62MS/MS

MS3

MS3

388.10 509.12

712.19

915.31

1077.36

1280.45

MS/MS%Int.

0

100

%Int.

15.0 20.0 25.0 30.0 35.0 40.0 45.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

TIC

1 23

4

5

6

7

8

9

1011

12

13

14

15

16

17

18

19

20

21

22

23

2425

26

27

28

293031

32

33

34

35

3637

38

39

40

(x1,000,000)

10.0 15.0 20.0 25.0 30.0 35.0 40.0 45.0

0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

1

4

7

8

12

15

20

21

26

29

31

3840

44

45

47

5056

5859

606368

707680

86

87

94

109

114116118122

135138

143

147

164

175

179

180181

182

183

184

185

186187

188

(x10,000,000)TIC


24/3424

Application

LCMS-8080

LCMS-IT-TOF

Two-dimensional LC/LCMS-IT-TOF systems can use unmodified HPLC purity test conditions. The first dimension separates impurities into

fractions in the fraction loop, then the fractioned impurities are injected into the second dimension LCMS system. The UV chromatogram in

Fig. 1 was created by using a 2-dimensional LC/LCMS-IT-TOF system to measure atorvastatin hydrates, which were added to the Japanese

Pharmacopoeia 16th revision.

Nineteen impurity peaks were detected in measurements, with 10 impurities having an area that is 0.1 % or more of primary components.

LCMS-8080 CYP cocktail assay: Reagents

This assay is standard method for checking toxicity and safety of drug candidates. P450 enzymes metabolizes toxin. The inhibition of drug

candidates is investigated by mixing substrates, P450 and drug and react enzyme.

The mixture of 5 substrates were metabolized in human liver microsome (=P450 enzyme) and then metabolites were quantified by LCMS-8080.

All five metabolites were successfully quantified even though their actual concentration ranging from 0.9 to 900nM.

The results with polarity switching experiment did not pale against the results with dedicated polarity.

The 20 msec polarity switching capability helps researchers need to grab the ultra high sensitivity and data quality.

Of the 19 impurities, impurity 2 has the smallest area value. This area was only 0.013 % the area of

primary components. A UV chromatogram, mass chromatogram, and mass spectra of impurity 2

measured using a 2-dimensional LC/LCMS-IT-TOF system is shown to the left.

Fig. 2 shows an overlay of UV chromatograms from the 2-dimensional LC/LCMS-IT-TOF system. The

impurities can be identified by comparing peaks to blank sample results. The mass spectra in Fig. 3

were integrated for the elution range for impurity 2.

A molecular mass of 573 is observed in the ESI- spectrum. This pre-

sumably corresponds to impurity 2, which has a molecular weight of

574. The 597 value in the ESI+ spectrum is a Na adduct ion. Even

though the impurity concentration was a trace 0.013 %, a mass spec-

trum with good sensitivity was obtained.

Fig. 1 First Dimension HPLC UV Chromatogram (254 nm)

Fig. 3 Mass Spectra of Impurity 2

Fig. 2 Second Dimension HPLCUV Chromatogram (254 nm)

0 10 20 30 40 50 60 70 min

0.0

0.5

1.0

1.5

mAU (x10)254nm,4nm (1.00)

Conc.0.013%

Impurity 2mpurity 2Impurity 2mpurity 2

4.25 4.50 4.75 5.00 5.25 5.50 min

3.0

4.0

5.0

6.0

uV (x100)

Sample

Blank

500 550 600 650 m/z0.0

1.0

2.0 573.2400 MS1 spectrumnegative

Inten. (x1,000,000)

500 550 600 650 m/z0.0

1.0

2.0

Inten. (x1,000,000)

557.2470

597.2381

613.2161

MS1 spectrumpositive

2-Dimensional LC/LCMS-IT-TOF System Capable of Using Mobile Phase Conditions Not Suited to MS analysis

Hydroxy tolbutamide (-)285.0>186.0

Oxidized nifedipine (+)345.0>284.0

(+/-)-4-Hydorxy mephenytoin (+)235.0>150.2

1-Hydroxy bufuralol (+)278.2>186.0

Resorufin (+)214.0>186.0

Substrates

Resorufin ethyl ether

Bufuralol hydrochloride

(S)-Mephenytoin

Nifedipine

Tolbutamide

Metabolites/Products

Resorufin

1-Hydroxy bufuralol

(+/-)-4-Hydroxy mephenytoin

Oxidized nifedipine

Hydroxy tolbutamide

P450 Enzyme

CYP 1A2

CYP 2D6

CYP 2C19

CYP 3A4

CYP 2C9

LOD / nM

0.01

0.21

0.37

0.002

0.003

LOQ / nM

0.6

0.6

0.6

0.6

0.6


25/34

MALDI-TOF MS

Analysis of Potential Genotoxic Impurit ies in Active Pharmaceutical Ingredients Using GCMS

GCMS

During the process of synthesizing active pharmaceutical ingredients, methanesulfonic acid (mesylate), benzenesufonic acid

(besylate), andp-toluenesulfonic acid (tosylate) can generate sulfonic acid esters as a reaction by-product. These compounds are

known to be potential genotoxic impurities (PGIs), which is a major concern to pharmaceutical manufacturers. Results from analyz-

ing sulfonic acid ester PGIs are shown below.

Total Ion Current Chromatogram

Structural Formula of Sulfonic Acid Esters

Ester methanesulfonate

Esterbenzenesulfonate

Ester-toluensulfonate

R: alkane

2.5 5.0 7.5 10.0 12.5

1.0

2.0

3.0

4.0

12

3

4

5 67

8

9

10 1112

TIC

(x1,000,000)

p

1 Methyl methanesulfonate2 Ethyl methanesulfonate3 Isopropyl methanesulfonate4 n-propyl methanesulfonate5 Methyl benzenesulfonate6 Ethyl benzenesulfonate

7 Methyl p-toluensulfonate8 Ethyl p-toluensulfonate9 Isopropyl p-toluensulfonate

10 Butyl benzenesulfonate11 n-propyl p-toluensulfonate12 Butyl p-toluensulfonate

ID Retention time Retention timeCompound name Compound nameID

3.0473.8644.2684.9858.6779.278

9.80110.34510.53610.88511.07111.828

MALDI-TOF MS imaging is a revolutionary new technology that provides images showing the distribution of molecules in biological tissue,

based on the signal intensities and masses of ions detected with a mass spectrometer. Therefore, it is possible to investigate the presence

and localization of drugs administered to animals, or their metabolic products, in tissue sections. It is expected to apply drug delivery and

pharmacokinetics research.

An ion at m/z327, which corresponds to

the mass of clozapine, is detected of

mass spectra on brain tissue section. The

ion was confirmed to be clozapine from

MS/MS analysis results. A mass image of

the detected clozapine (figure (c) on the

left) shows that clozapine is detected in

a variety of locations throughout the

brain t issue section, but it is strongly

de tected espec ia l l y in the ce rebra l

cortex.

In contrast, the distribution of demethyl-

ated clozapine differs from clozapine

(figure (d) on the left).

Pharmacokinetic Applications (mass imaging of brain tissue sections)

(a) Diagram of Dissected Rat Brain Tissue

(c) Mass Image of Clozapine (m/z327)

Ion intensity scale:

(d) Mass Image of Demethylated Clozapine (m/z313)

(b) Rat Brain Tissue Section(optical microscope image with H&E staining)

1 Cerebral cortex2 Cerebellum

3 Midbrain4 Fornix5 Thalamus6 Septum

7 Olfac tory bulb8 Pons

9 Medulla oblongata10 Hypothalamus11 Spinal cord12 Pituitary gland

12 3 4

5 6 7

89 1012

11


26/3426

Food Safety

LCMS-8030

Analysis of Veterinary Drugs Using Method Packages

As concern grows for food safety and the ecology, the number of substances regulated to protect our lifestyles continues to increase.

Consequently, there is now an increased needs for an easier inspection method and faster multiple components simultaneous analysis.

Therefore, more LC/MS/MS systems are being utilized in recent years, due to sample pretreatment requirements that can be made

shorter than using GC/MS systems.

Using an LC/MS/MS Method Package allows starting quantitative analysis quickly by simply confirming separation parameters, without

having to optimize MS parameters for each compound required before starting LC/MS/MS analysis. Each type of method package

includes simultaneous analysis method files, a list of MRM transitions, and report templates. Measurement methods can be completed

by simply selecting text files for necessary components from the list of MRM transitions and correcting retention times by analyzing a

standard sample.

Multi-class pesticides analysis in vegetable using ultra fast LC/MS/MS and GC/MS/MS

Many regulatory authorities have established multi-class residual pesticides methods for the analysis of vegetables, fruits

and other food stuffs. There is, however no global agreement on the provision of a target list of pesticides and this presents

a risk with products moving between different regulatory requirements. In order to eliminate this risk, food safety laborato-

ries need to ideally screen as many compounds as possible in a single run which may reach maximum residual limits (MRL);

typically 10 ppb in food matrices. In this study, we report the application of ultra-fast 5 msec MRM with 15 msec polarity

switching for the analysis of 138 pesticides in vegetable matrices (72 and 66 compounds measured by LC-QqQ and GC-QqQ

in the European Union Reference Laboratory (EURL) method). Approximately 90% of pesticides represented good recover-

ies in the range of 70-120% in all studied matrices.

LCMS-8040 / GCMS-TQ8030

Method Package (MS Parameters)for Veterinary Drugs

Method Package(LC Parameters) for Veterinary Drugs

MRM Chromatograms of Veterinary Drugs

1.0(1,000,000)

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

0.1

0.05.0 10.0 15.0 20.0 25.0 30.0 35.0 min

HPLC

Column

Mobile Phase A

Mobile Phase B

Gradient Program

Flow Rate

Column Temperature

Shim-pack HR-ODS

(3.0 mmI.D. x 150 mmL., 3 m)

0.1% Formic acid - water

Acetonitrile

1 %B (0 min) - 100 %B (35-40 min)

- 1 %B (40.01 - 50 min)

0.4 mL / min

40C

Compounds for LC-QqQ Compounds for GC-QqQ

1-1000 ppbr2=0.9999

S/N 381 ppb

S/N 821 ppb

S/N 731 ppb

S/N 731 ppb

1-1000 ppbr2=0.9992

1-1000 ppbr2=0.9999

1-1000 ppbr2=0.9996

0 500 Conc.0.0

1.0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

Areax10,000,000

Azoxystrobin Carbofuran Ethion Methidathion

0 500 Conc.

0.00

0.25

0.50

0.75

1.00Areax100,000,000

0 500 Conc.0.0

2.5

5.0

7.5

Areax10,000,000

0 500 Conc.0.0

2.5

5.0

7.5

Areax10,000,000

5.0 6.0

0.0

0.5

1.0

1.5

2.0x100,000

0.00

0.25

0.50

0.75

1.00

1.25

1.50

1.75

2.00x100,000

9.0 10.0 6.0 7.0

0.00

0.25

0.50

0.75

1.00

1.25

1.50

1.75

x100,000

6.0 7.0

0.00

0.25

0.50

0.75

1.00

1.25

1.50

1.75

2.00x100,000

1 ppb

5 ppb

10 ppb

Azoxystrobin

5 ppb standards spiked

Matrix blank

ClothianidinImidacloprid

Azoxystrobin

8.19 ppb

3.77 ppb

5 ppm

Imidacloprid

8.99 ppb

3.19 ppb

3 ppm

Clothianidin

25.78 ppb

21.39 ppb

15 ppm

Fludioxonil

556.58 ppb

550.92 ppb

10 ppm

5 ppb standards spiked

Matrix blank

MRLJapan

Fludioxonil

6.5 7 .0 7 .5

0

50000

100000

150000

200000

250000

300000

3.5 4.0 4.5

0

10000

20000

30000

40000

50000

60000

70000

80000

3.5 4.0 4.5

0

2500

5000

7500

10000

12500

15000

17500

20000

6.0 6.5 7.0

0

25000

50000

75000

100000

125000

150000

4MRM4MRM5 ppb


27/34

AXIMA

GCMS

Analys is of Res idua l Pest ic ides in Food Us ing Twin L ine-GC/MS

The fastest and easiest microorganism identification by MALDI-TOFMS

By using a twin line system, two columns can be installed in a GC-MS. Switching between the columns is accomplished simply by changing

settings. To analyze pesticides in foods, two columns with different types of solid phases were installed using the twin lines. By comparing

the results obtained from each column, reliability can be increased for both quantitative and qualitative analysis. In particular, if a pesticide

overlaps with an impurity, in some cases the second column enables separation with a different type of solid phase. Therefore, comparing

data from two columns makes data analysis easier and improves reliability.

When MALDI-MS spectra are measured directly on microorganism like bacteria, mainly several dozens of ribosome proteins are detected. MS

spectrum pattern is dependent on microorganism species, because the amino acid sequence of ribosome protein is different each species.

By storing those MS spectra in database just for MALDI-TOFMS and identification, three steps microorganism ID are enabled without compli-

cated sample preparation. High throughput analysis, a thousand sample run per day, is capable 1). By compiling many data, which are

acquired with varying strains and culture conditions, as a mass spectrum of a species in database, incorrect rate can be reduced and microor-

ganism ID can be stable. Figure 2 shows identification results of Trichophyton rubrum isolates.

Total Ion Chromatograms Using Columns with Different Types of Solid Phase (1 g/mL of 97 types of pesticides)

Rtx-5MS Rtx-OPPesticides2

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5

0.5

1.0

1.5

2.0 TIC

(x10,000,000)

5.0 7.5 10.0 12.5 15.0 17.5 20.0 22.5 25.0 27.5

0.5

1.0

1.5

2.0

2.5

TIC

(x10,000,000)

Identification of unknown samples: matching mass

fingerprints to database

1) Time for measurement and identification is dependent on measurement parameters and sample condition.

Schematic Overview of Identification of Microorganisms

Using MALDI-TOF MS

1.Sample preparation

Bacterial cells spotted on

MALDI sample plate and

mixed with matrix reagent

MS fingerprints of bacterial

samples are automatically

acquired using MALDI-TOF MS

Matching fingerprints

of the samples to database

Upper: MS spectrum of Trychophyton rubrum in Database Middle and

Lower: Mass spectrum of two clinical isolates .

Both isolates were identified as Trichophyton rubrum.

2.Mass analysis 3.Matching fingerprint


28/3428

Food ingredients alalysis

LCMS-8040 / LCMS-8030

Analysis of Geniposidic Acid and Chlorogenic Acid in Tochu Tea

LCMS-8040 / LCMS-8030

A B

2.0 3.0 4.0 min min

0

250

500

750

1000

1250

1500

1750

2000373.00>123.30(-)

Ge

niposidicacid/3.4

51

6.0 7.0 8.0 9.0

0

2500

5000

7500

10000

12500

15000

17500

20000

22500

25000

27500

30000 353.00>191.20(-)

Chlorogenicacid/7.6

22

Analysis of Water Soluble VitaminsOn August 24, 2007, the U.S. Food and Drug Administration (FDA) published cGMP (Current Good Manufacturing Practice) in Manu-

facturing, Packaging, Labeling, or Holding Operations for Dietary Supplements, 21 CFR (Code of Federal Regulations) Part 111. This

regulation mandates testing the ingredients in supplements. The following shows an example of using LC/MS/MS to quantitatively

analyze water soluble vitamins in a commercial dietary supplement. Nine water soluble vitamins were measured with good separation

and sensitivity. In addition, each ingredient was successfully quantitated in a supplement extract solution without being affected by

contaminant components. Quantitation results are shown below.

Tochu tea, made from the leaves of tochu (Eucommia ulmoides), is one of the five most popular Chinese herbal medicines. Tochu tea

is rich in the iridoids geniposidic acid and chlorogenic acid (3-caffeoylquinic acid), and the antihypertensive effects of geniposidic acid

is well known. LC/MS has been employed in recent years to analyze the polyphenols in these plant extracts. MRM chromatograms of

geniposidic acid and chlorogenic acid in the 1,000 to 1 diluted tochu tea is shown (Fig. 1). Analysis was accomplished without signifi-

cant interference from impurity components. The 1,000 to 1 dilution of tochu tea contained approximately 600 to 700 ppb genipo-

sidic acid and chlorogenic acid.

MRM Chromatograms

of Water Soluble Vitamins

Calibration Curves

of Water Soluble Vitamins

MRM Chromatograms and Quantitation Results for

Commercial Supplement Extract Solution

MRM Chromatograms of Geniposidic Acid (A) and Chlorogenic Acid (B) in Tochu Tea

1:265.10>122.10(+)(0.80)

2:170.10>152.20(+)(0.50)

3:124.20>80.0(+)(5.00)

4:123.10>80.0(+)(0.60)

5:220.10>90.00(+)(1.60)

6:678.55>146.80(+)(9.00)

7:377.20>242.80(+)(10.00)

8:245.10>227.10(+)(0.80)

9:440.20>295.10(+)(10.00)

Thiamin

Pyridoxine

Nicotinicacid

Nicotinamide

Pantothenic acid

Cyanocobalamin

RiboflavinBiotin

Folicacid

0

0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 min

500000

1000000

1500000

2000000

Thiamin

Cyanocobalamin Riboflavin

Pyridoxine

0 250

Area (x100,000)

Area (x100,000) Area (x10,000)

Area (x1,000,000)

0.5500 ng/mLR2 = 0.9999

5010,000 ng/mLR2 = 0.9992

1500 ng/mLR2 = 0.9993

101,000 ng/mLR2 = 0.9999

7.5

5.0

2.5

0.0

Conc. 0 250 Conc.

1.00

0.75

0.50

0.25

0.00

4.0

3.0

2.0

1.0

0.0

2.0

1.0

1.5

0.5

0.0

0 5000 Conc. 0 500 Conc.

Thiamin PyridoxineArea (x100,000) Area (x100,000)

Area (x100,000)Nicotinamide

0

0.5

1.0

1.5

1.50 2.00 2.50 min

15.6 mg

0

1.0

2.0

2.50 3.00 3.50 min

11.0 mg

0

1.0

2.0

3.0

4.0 43.4 mg

4.00 5.00 min

Compound

Thiamin

Pyridoxine

Nicotinic acid

Nicotinamide

Pantothenic acid

Cyanocobalamin

Riboflavin

Biotin

Folic acid

Quantitation Results (forabout10 tablets)

15.6 mg

11.0 mg

0 mg

43.4 mg

20.6 mg

23.3 g

6 mg

35.6 g

218.4 g


29/34

GCMS

LCMS-2020

DART (Direct Analysis in Real Time) is the atmospheric pressure

ionization method, which is easy and useful for analyzing the

molecules in food without pretreatment. DART ionizes multi-

component in a moment and LCMS-2020/8030/8040 ultra fast

polarity switching and ultra fast scanning function allows mul-

ticomponent direct analysis in food. This data is the analysis

results of soy-source and fish source in different producing

district and raw material, and this shows the difference of spec-

tra pattern owing to amino acid balance in each raw material.

GCGC is state-of-the-art chromatography technology that involves directly connecting two different columns together to achieve

high separation levels. GC Image was used to create two-dimensional results from analyzing diesel fuel using a GCGC-MS system,

as shown to the left. A column with high polarity was used for the second column, which enabled separating aromatic hydrocar-

bons, which tend to overlap with paraffins. These can be detected as a blob distribution pattern that reflects the compound struc-

ture.

Componential Analysis Using DART-MS of Ultra-Fast Polarity Switching

0.0

1.0

2.0

3.0

Inten.(x100,000)

115.75

228.80137.80 252.8069.80

100 200 300 400 m/z

100 200 300 400 m/z

100 200 300 400 m/z

100 200 300 400 m/z

100 200 300 400 m/z

0.0

1.0

2.0

Inten.(x100,000)

115.75

230.80

198.75146.7569.85

0.0

0.5

1.0

Inten.(x100,000)

115.75

226.80

146.80 196.80

69.75

0.0

0.5

1.0

Inten.(x100,000)

111.75226.80

88.80

71.85 196.85

240.85

0.0

0.5

1.0

1.5

Inten.(x100,000)

113.75 226.80

172.8059.85

259.7583.80 199.80 449.95

Positive

0.0

2.5

Inten.(x100,000)

187.10

217.10128.10

189.10

117.10164.10238.15

384.1089.1551.30

475.10

0.0

1.0

2.0

3.0

Inten.(x100,000)

217.10

187.10

128.15 189.10238.10 289.10164.05 384.20

51.25117.15

0.0

1.0

2.0Inten.(x100,000)

217.15

202.15128.15

236.10146.15

384.2051.55

117.10

0.0

1.0

2.0

3.0Inten.(x100,000)

217.10

202.20128.15 418.10

51.95 480.15

100 200 300 400 m/z

100 200 300 400 m/z

100 200 300 400 m/z

100 200 300 400 m/z

100 200 300 400 m/z

0.0

1.0

2.0

3.0

Inten.(x100,000)

128.15

164.10117.15

166.1089.15 257.1551.40

209.10 369.95

A

B

C

K

N

Negative

Analysis of Diesel Fuel Using GCGC-MS

2-Dimensional Image of GCGC-MS Analysis Results for Diesel Fuel

DART-SVP ion source and LCMS-2020 DART is a product of IonSense Inc. (http://www.ionsense.com/).

Analysis results of several kinds of soy-sourceand fish source by DART-MS


30/3430

Chemical

LCMS-8030

Analysis of Additives in Polymer Extract Solution Using LCMS-IT-TOF

Mass Chromatogram of Plastic Plate Extract by Synchronized Survey Scan

LCMS-IT-TOF

It is known that the additives added to polymer materials can vary even for identical types of products, depending on the grade or manufac-

turer. Therefore, identifying the additives in polymer materials provides important information for investigating the performance of competi-

tor products or improving one's own products.

Based on the formula (C28H52N2O4) predicted for peak A using Formula Predictor and accurate masses obtained from MS, MS/MS, and

MS/MS/MS analysis, peak A presumably corresponds to decanedoic acid bis (2,2,6,6-tetramethyl-4-piperidyl) ester.

Analyzing the additives in polymer materials is extremely important

for investigating the performance of different polymer materials

and for making product improvements. An example of measuring a

plastic plate extract using the ultrafast polarity switching, ultrafast

scanning performance, and Synchronized Survey Scan function

offered on the LCMS-8030 is shown.

Based on the detected masses and MS/MS spectra, it was

determined that the plastic plate contains Irganox 245, Tinuvin P,

and Cyanox 425. These results also suggest it contains other

additives as well.

UV Chromatogram and Mass Chromatogram

Peaks A, B, C, and E were detected using ESI+ ionization, whereas Peak D was detected using ESI-.

Mass Chromatogram of Plastic Plate Extract by

Synchronized Survey Scan

Mass Spectra of Peaks at an Elution Time of 2.82 Minutes

HPLC/UV

Mass chromatogram

A

B

C

D

E

(x1,000,000,000)

Detector A

0

Tinuvin P

Irganox 245

Cyanox 425

(100,000,000)

4.0

3.0

2.0

1.0

0.0 1.0 2.0 3.0 4.0 5.0 6.0 min

Q3 Scan TIC(+)

Q3 Scan TIC(-)

HO

O

OO

O

O

O

OHIrganox 245MW 586.7

250 500 m/z

Inten.(x1,000,000)

0.0

2.0

1.0

585.4

717.3

Q3 Scan (-)

0.0

2.0

3.0

1.0

250 500 m/z

234.6367.0

585.3

Inten.(x100,000)Product Ion Scan (-)

250 500 m/z

Inten.(x100,000)Product Ion Scan (-)

367.0233.3

149.3

82.9

41.5

0.0

1.0

0.5


31/34

AXIMA

Analysis of Diesel Fuel Using GCGC-MS

Analysis of Polyethylene Terephthalate (PET) Oligomer Using SEC-MALDI

GCMS

GCGC is state-of-the-art chromatography

technology that involves directly connecting two

different types of columns together to achieve

high separation levels. GC Image was used to

create two-dimensional results from analyzing

diese l fue l us ing a GCGC-MS system, as

shown to the left. A high polarity capil lary

column was used for the second column sepa-

rated aromatic hydrocarbons, which tend to

overlap with paraffins. These can be detected as

a blob distr ibution pattern that reflects the

compound structure.

Soxhlet extraction or precipitation methods

are used to pretreat samples for oligomer

analysis, and HPLC, NMR, or MALDI-TOF

MS (particularly more recently) systems are

used for detection.

However, polymer materials are, by

definition, a mixture of multiple compo-

nents, which means small amounts of

components cannot be detected by simply

analyzing the extract with mass spectrom-

etry. Using this system, which combines

size exclusion chromatography (SEC) withMALDI-TOF MS, enables detailed oligomer

analysis.

An example of using this system to analyze

a recycled PET product is shown.

Compared to oligomers in standard PET

polymers, a relatively broader distribution

of molecular weights was obtained and

more linear type oligomers were detected

from the recycled item.

: -(m/n)-; linear oligomers

(m/n); cyclic oligomers

m; Number of terephthalic acid (TA) units

n; Number of ethylene glycol (EG) units

Legend

2-Dimensional Image of GCGC-MS Analysis Results for Diesel Fuel

Recycled PET (cleaning utensil)

Elution Time


32/3432

LCMS-8030

Screening Analysis of Golf Course Pesticides

Analys is of Carbamate Pest ic ides Us ing Prominence UFLC and LCMS-2020

LCMS-IT-TOF

Environmental

The LCMS-8030 was used to simultaneously analyze 21 of the pesti-

cide components subject to evaluation by LC/MS, as specified in the

Provisional Guidance Indicators for the Prevention of Water Pollution

from Pesticides Used in Golf Courses, published by Japan's Ministry

of the Environment on September 29, 2010.

Good linearity was obtained for all the components in the range of

0.5 to 100 g/L.

If multiple components need to be analyzed simultaneously, it may be difficult to achieve full separation using HPLC alone. The high

selectivity offered by mass spectrometers is especially useful in such cases. The figure below shows an example of results from analyz-

ing carbamate pesticides. Even at low 500 ppb concentrations, the mass spectrometer provided more than adequate detection sensitiv-

ity. Furthermore, high throughput can be achieved for processing multiple analytes by combining it with a UFLC system.

MRM Chromatogram of Golf Course Pesticides

Calibration Curves forRepresentative Golf Course Pesticides

0 50

3.0

2.0

1.0

0.0

Conc.

Acetamiprid

Area (x1,000,000)

0.5-100 g/LR2=0.9998

3.0

4.0

2.0

1.0

0.0

0 50 Conc.

0.5-100 g/LR2=0.9998

Area (x1,000,000)

Isoxathion

0

2.0

3.0

4.0

5.0

6.0

7.0

8.0

9.0

10.0

11.0

12.0

13.0

14.0

15.0

16.0

17.0

(1,000,000)

1.0

0.0 2.5 5.0 7.5 10.0 12.5 15.0 min

292.00>211.10 (+) Thiamethoxam

223.05>126.05 (+) Acetamiprid

435.05>182.00 (+) Harosulfuron-methyl

399.10>261.00 (+) Ethoxysulfuron

202.10>124.15 (+) Simazine

422.05>261.05 (+) Cyclosulfamuron

280.00>220.15 (+) Metalaxyl

404.10>372.05 (+) Azoxystrobin

270.05>119.10 (+) Mepronil

303.05>185.15 (+) Cumyluron

308.10>70.05 (+) Tebuconazole

342.00>69.10 (+) Propiconazole

305.05>169.15 (+) Diazinon

333.05>180.15 (+) Butamifos

314.00>105.05 (+) Isoxathion

329.05>125.10 (+) Pencycuron

346.05>278.15 (+) Triflumizole

376.05>190.20 (+) Oxaziclomefone

331.05>181.15 (+) Pyributicarb

254.10>228.05 () Propyzamide

396.10>213.10 () Bensulide

1: Aldicarb sulfoxide

2: Aldicarb sulfone

3: Oxamyl

4: Methomyl

5: Methiocarb sulfoxide

6: 3-OH Carbofuran

7: Methiocarb sulfone

8: Aldicarb

9: Bendiocarb10: Carbofuran

11: Carbaryl

12: Thiodicarb

13: Ethiofencarb

14: XMC

15: Pirimicarb

16: Isoprocarb

17: Trimethacarb

18: Fenobcarb

19: Methiocarb

20: Benfuracarb

1

2

8

10

11

13

2017

1918

14

15

3 4 5

6

7

9

16

12

207.00(60.47)

240.00(8.47)

237.00(14.56)

163.00(16.38)

242.00(8.49)

220.00(50.06)

239.00(1.20)

258.00(67.41)

222.00(3.94)

224.00(9.71)

208.00(6.66)

226.00(7.43)

202.00(27.56)

355.00(5.65)

180.00(9.38)

194.00(5.73)

411.00

TIC

(x10,000,000)

1.00

0.75

0.50

0.25

0.00

1.50 1.75 2.00 2.25 2.50 2.75 3.00 3.25 3.50 3.75 4.00 4.25 min


33/34

ASMS

Measurement of Contaminants in River Water Using Compound Composer Database Software for Simultaneous Analysis

GCMS-TQ8030

Environmental analysis involves monitoring target compounds, but it is also important to verify the presence and approximate concentration

of non-target hazardous substances. Therefore, it is important to perform a simple and rapid screening process to analyze as many

applicable chemical substances as possible. Compound Composer Database Software for Simultaneous Analysis provides an easy way to

screen for hazardous chemicals without the use of standard samples. Measuring contaminants in river water, it enabled detecting low

concentrations of pharmaceuticals and personal care products (PPCPs), such as crotamiton and L-menthol, which have gained attention in

recent years, bisphenol A, nicotine, and caffeine.

Results from River Water Analysis

Bisphenol A was detected automatically and a semi-quantitative result was obtained without using a standard sample.

Spectrum of unknown components

Registered spectrum

Quantitation graphID#:2 m/z:213.00Type: TargetCompound name:2;3;0;Bisphenol A

Retention time:26.332Area:7943

Similarity:84Concentration:0.0723ug

#2 Retention time: 26.3 (Scan #: 4667)Number of peaks:265Spectrum average:26.3-26.3(4666-4668)Background: Group 1 - Event 1 calculated from peaks

Spectral graph

The Screening Analysis of PCBs in transformer oil by Using Neutral Loss Scan of GC/MS/MS

Neutral loss scan selectively detects precursor ions with a specific neutral loss and used for the screening analysis compound family, which

includes common partial molecular structure or residues. For example, neutral loss scans at m/z35 and 37 are representative of com-

pounds containing chlorine. PCBs were spiked to transformer oil and PCBs screening analysis were performed by neutral loss scans of

chlorine.

Chromatogram of Transformer Oil Spiked with PCBs

Black: Scan mode

Red: Neutral loss scan mode

Scan measurement and similarity search of peaks

detected by neutral loss scan

Measured spectrum

Library spectrum


34/34

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