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Application of Gas chromatography Mass Spectrometry (GC MS) in

Food Science and Biotechnology

Presentation · June 2014

DOI: 10.13140/RG.2.2.35663.07844

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 Application of Gas chromatography Mass Spectrometry (GC MS) in Food Science and Biotechnology

Application of Gas chromatography Mass

Spectrometry (GC MS) in Food Science and
Biotechnology
Assist. Prof. Dr. Dhia Falih Al-Fekaiki
Director of chromatography analyses Lab.
alfekaiki@yahoo.com
Iraq- Basrah
 Gas chromatography mass spectrometry (GC/MS)

Gas chromatography mass spectrometry (GC/MS) is an instrumental technique,

comprising a gas chromatograph (GC) coupled to a mass spectrometer (MS), by which
complex mixtures of chemicals may be separated, identified and quantified.

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 How GC/MS works - two part analysis
1-The GC separates mixes of chemicals into individual components
2-The MS fragments the chemicals into unique patterns or spectra.

Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 • Uses of GC MS
• Identification and quantitation of volatile and semi volatile organic compounds
in complex mixtures
• Determination of molecular weights and (sometimes) elemental compositions of
unknown organic
• compounds in complex mixtures
• Structural determination of unknown organic compounds in complex mixtures
both by matching
• their spectra with reference spectra and by a priori spectral interpretation
• Analysis Time
• In addition to sample preparation time, the instrumental analysis time usually is
fixed by the duration of the gas chromatographic run, typically between 20 and
100 min

Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015
 As the individual compounds elute from the
GC column, they enter the electron
ionization (mass spec) detector. There, they
are bombarded with a stream of electrons
causing them to break apart into fragments.
These fragments can be large or small pieces
of the original molecules.

Figure 1: Chromatogram generated by a GC.

The computer records a graph for each scan.

The x-axis represents the M/Z ratios. The y-
axis represents the signal intensity
(abundance) for each of the fragments
detected during the scan. This graph is
referred to as a mass spectrum (

Figure 2: Mass-spectrum generated by an MS.

 GC MS
In
Food Adulteration

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

• GC/MS Analysis of Melamine in Milk Powder
Determination and quantification by GC-MS of melamine (1 mg/kg)

Milk adulterationwith melamine in China

The 2008 Chinese milk scandal was a food safety

incident in China, involving milk and infant formula,
and other food materials and components,
adulterated with melamine.

China reported an estimated 300,000 victims with

six infants dying from kidney stones and other
kidney damage, and an estimated 54,000 babies
being hospitalized
 Analysis of Acrylamide in Food by GC–MS

Acrylamide in Food and Cancer Risk

Acrylamide is a chemical produced naturally in food as a result
of cooking starch rich food at high temperatures,
Highest Research
Food Finding for
Acrylamide Content

Grain-based coffee
5.399 ppm
substitutes
Potato chips 9270 ppb
French fries 1.325 ppm
Dehydrated onion
1.184 ppm
soup mix
Toasted wheat cereal 1.057 ppm
Cookies 0.995 ppm
Cocoa 0.909 ppm
• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015
• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015
 Polycyclic aromatic hydrocarbons (PAHs) in smoked fish from three smoke-
houses in Brasov county
GC–MS analysis.The Agilent 6890 gas
chromatograph equipped with an autosampler
7683 was connected to an Agilent 5975 mass
selective detector. 1 mL of sample solution was
injected in the pulsed splitless mode onto a 30m x
0.25mm i.d. DB-17 ms coated fused silica column
with a film-thickness of 0.15 μm. Other operating
conditions were: pulse pressure 45 psi, pulse time
0.90 min, purge flow 50mL, purge time 1.00 min;
helium carrier gas constant flow 1.1 mL/min;
temperatures: injector 300 0C, oven programme
700C for 1min, rate 200C/min-1600C, rate 30C/min-
2100C, rate 50C/min-final temperature 3200C, hold
for 5min, transfer line 3100C. MS conditions:
electron impact positive ion mode, detection
SIM.MS Source 2600C and MS Quad 1700C. The
GC-retention times and MS quantifying ions of
PAHs and internal standards are listed in Table
1.A calibration curve for each PAH was obtained
by running standards 5, 10, 20, 50, 100 and 200 ng
of each PAH and 200 ng of the appropriate internal
standard per mL cyclohexane.
 Analysis of arsenic species in fish after derivatization by
GC-MS.
Richter J, Lischka S, Piechotta C
Talanta. 2012 Nov 15;101:524-9. doi: 10.1016/j.talanta.2012.10.021. Epub 2012 Oct 12.

• The derivatization of organoarsenic compounds by different reagents like thioglycolates or

dithiols and the subsequent analysis by GC-MS as a molecular specific technique was
investigated and described. The possible derivatization reagents methyl- and ethylthioglycolate
(TGM and TGE), 1,3-propane- and 1,5-pentanedithiol (PDT and PeDT), which transfer the polar
and nonvolatile analytes dimethylarsenate (DMA), monomethylarsonate (MMA), arsenite and
arsenate into volatile compounds, were evaluated. The application for real samples like fish
material was also studied. In addition the gas chromatographic separation and resolution was
optimized and experiments were carried out to determine the highest derivatization rates.
Derivatization reagents were evaluated in terms of quantity and stability of the formed chemical
species. All derivatization products were characterized by mass spectrometry in order to identify
the separated arsenic species. The most efficient conversion of DMA and MMA was observed by
using ethylthioglycolate as derivatization agent. Finally, the derivatization procedure and the GC-
MS-method were validated to determine linearity, precision, selectivity, analytical limiting values
and recoveries. For the proposed method a limit of detection (LOD) of 5.8 pg for DMA and 14.0
pg for MMA was found. The accuracy was established by comparing the mean value measured
for DMA in the certified reference material BCR-627 (tuna fish) with the certified one. MMA was
not quantified in marine samples due to its low content. In shrimp samples DMA was not
detectable. For codfish a DMA-content of 0.20±0.004 mg kg(-1), for "Surströmming" an amount
of 0.38±0.02 mg kg(-1) and for herring, which showed the highest amount of DMA, a content of
1.15±0.03 mg kg(-1) was determined.

• Copyright © 2012 Elsevier B.V. All rights reserved

• .
 Identification of Essential Oil Components by
GC-MS
• At Aromatics International every batch of oil purchased from a distiller or
distributor is tested with GC/MS

• This process is used to identify any adulteration of the essential oil

tested and Purity

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

Detection 61 compounds in cumin essential oil by gc ms
Detection 54 compounds in crwa essential oil by GC MS
Detection 55 compounds in fennel essential oil by GC MS
Detection 46 compounds in anise essential oil by gc ms
We can distinguish between isomers by using GC MS

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 GC-MS analysis of Fatty acids

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 omega 3 fatty acid
• Fourteen individual fatty acids were identified using GC-MS technique
• Comparative analysis of EPA and DHA in fish oil nutritional capsules by GC-MS
 omega-5 long

Punicic acid is an omega-5 long

chain polyunsaturated fatty
acid found in pomegranate
seed oil.

(α-linolenate or 18:3(n-3)
 cyclopropane fatty acids
• Identification of cyclopropyl fatty acids in walnut
• Characterization and analysis of the cotton cyclopropane

• The formation of cyclopropane fatty acids in Salmonella enterica serovar

Typhimurium
 Determination of amino acids

• Quantification of D-amino acids in human urine using GC-MS

• Amino Acids Determination in Meat by GC-MS
• Qualitative amino acid analysis of small peptides by GC/MS.
• GC-MS analysis of t-BDMS derivatives of amino acids
GC-MS uses to Detection and Identification the
Antioxidant Compounds
Gas Chromatography-Mass Spectrometry (GC-MS) and evaluation
of antioxidant and antimicrobial activities of essential oil of
Campomanesia adamantium (Cambess.) O. Berg (Guavira)

Volatile Compounds and Antioxidant Capacity of the Bio-Oil

Obtained by Pyrolysis of Japanese Red Pine (Pinus Densiflora
Siebold and Zucc.)

Antioxidant and Antimicrobial Activities with GC/MS

Analysis of the Morus alba L. Leaves
GC-MS ANALYSIS OF PHYTOCOMPONENTS AND TOTAL ANTIOXIDANT
ACTIVITY OF HEXANE EXTRACT OF SINAPIS ALBA

Butylated Hydroxytoluene in Edible Vegetable Oils

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 GC-MS uses to Detection and Identification the
ANTIMICROBIAL Compounds
• SCREENING OF ACTIVE PHYTOCOMPOUNDS BY GC – MS STUDY AND ANTIMICROBIAL

• EVALUATION OF ANTIMICROBIAL METABOLITES FROM MARINE MICROALGAE

TETRASELMIS SUECICA USING GAS CHROMATOGRAPHY – MASS
SPECTROMETRY (GC – MS) ANALYSIS

• GC/MS analysis and antimicrobial activity of the essential oil of fresh leaves of
Eucalytus globulus
• GC/MS Analysis of Melamine in Milk Powder

• determination of volatile compounds in cows' milk using headspace GC-

MS.
Forty-one compounds in milk were isolated and identified from GC-MS headspace
analysis.

• Determination of Veterinary Drug Residues in Milk by GC/MS

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 Volatile Compounds in Honey

IDENTIFICATION OF HONEY VOLATILE COMPONENTS BY SOLID PHASE

MICROEXTRACTION (SPME) AND GAS CHROMATOGRAPHY/MASS SPECTROMETRY
(GC/MS)

A new methodology based on GC-MS to detect honey adulteration with

commercial syrups.

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

 GC/MS Analysis of Phthalates in Children’s Products

Plastic is a well suited material for the manufacture of a wide

range of products. Children’s products, from plates and cups to
mattress liners and diapers and toys, are made of plastic,as a result
of its low cost and durability. The manufacture of plastic products
often includes additives which are intended to modify the physical
properties of the polymer. Common additives are plasticizers,
antioxidants and flame retardants. There are a num- ber of
different compounds classified as plasticizers – the most common
are
• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015
Graduate student
Matt Limmer uses the
SPME, or solid-phase
microextraction fiber,
to extract a sample
from a tree in
Schuman Park.
Clinical Application of SPME: Analysis of volatile organic
compounds (VOCs) in Exhaled Breath as Cancer Biomarkers

1. Ethanol
2. Acetonitrile
3. Acetone
4. 2-Propanol
5. Isoprene
6. Pentane
7. Methacrolein
8. Methyl vinyl ketone
9. Ethyl acetate
10. 2-Methylpentane
11. 3-Methylpentane
12. Hexane
13. Toluene
14. Hexanal
15. Limonene
Solid-phase micro-extraction (SPME) sample collection
SPME experiments were performed at ambient temperature. A mouse carcass (laboratory
mice, Mus musculus) was placed on a glass rectangular plate (10 cm × 10 cm) and covered
with an oval glass cover lid (10 cm dia, 7 cm height). The centre of the glass lid protrudes up
to form a standard glass screw joint (8 mm dia). The joint was closed using a corresponding
plastic cap with a PTFE septum. The SPME holder with CAR/PDMS fibre (Supelco, previously
desorbed for 5 min in GC injection port heated to 200 °C) was inserted through the PTFE
septum into the atmosphere surrounding the mouse carcass and the fibre was exposed for 15
min and immediately GC×GC-TOFMS analysed. 10 mouse carcasses (Mus musculus) were
used. During the first 24 h, SPME samplings were performed at every hour. Later on,
samplings were repeated at longer intervals

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

Analysis of Pesticides in Food Matrix by GC/MS/MS
 Analysis of Dithiocarbamate Pesticides by GC-MS
The class of dithiocarbamate fungicides (DTCs) is widely used in agriculture. They are
non-systemic and both the formulation and their break-down products typically
remain at the site of application. DTCs are characterized by a broad spectrum of
activity against various plant pathogens, low acute mammal toxicity, and low
production costs The dithiocarbamate moiety is highly reactive: it readily chelates
most heavy metals, reacts with sulfhydryl groups of proteins, rendering itself
neurotoxic, teratogenic, and cytotoxic.
The Application of GC/MS to the Analysis of Pesticides in Foodstuffs
 Multi-Residue Pesticides Analysis in Herbal Tea Products by GC-MS
The residue analysis of pesticides has developed in recent years into a comprehensive
methodology for the detection of many hundreds of potentially food contaminating
compounds. A multi-residue method for teas and herbal products in general is faced
withThe residuechallenges
particular analysis ofwith
pesticides
the highhas developed
number in recentdue
of pesticides years
to into a comprehensive
a worldwide origin
methodology for the detection of many hundreds of potentially
of the products and the complex matrix of the dried plant materials. food contaminating
compounds.
In the due qualityAcontrol
multi-residue method forthe
of raw materials, teas and herbal
unknown products inlocal
or undeclared general
plantis faced
with particular
protection treatmentchallenges
has to bewith
takenthe high
into number
account of pesticides
with due of
a wide variety to potential
a worldwide origin
of thecontaminations.
pesticide products and the Thecomplex matrixfruits
dried leaves, of theordried
seeds plant
and materials.
other medical products
In the
deliver duecomplex
highly quality control
extractsoffrom
raw the
materials,
samplethe unknown due
preparation or undeclared
to the rich local
contentplantin
protection treatment has to be taken into account with a wide variety
active ingredients, essential oils and the typical high boiling natural polymer of potential
pesticidefrom
compounds contaminations.
broken cells, The dried
leaves leaves,
or fruit fruits or seeds and other medical products
skins.
deliver highly complex extracts from the sample preparation due to the rich content in
active ingredients, essential oils and the typical high boiling natural polymer
compounds from broken cells, leaves or fruit skins.
Tandem GC/MS Analysis of Pesticides in. Food Oils by Large Volume Injection

Analysis of Pesticide Residues in Apple using

 Determination of Quinolone Residues in Bovine Liver

A method for the determination of 11 Quinolone antibiotics in bovine liver has been
established:
The quinolones are a family of synthetic broad-spectrum antibacterial drugs
 DNA damage
Measurement of oxidative DNA damage by gas chromatography-mass spectrometry:
ethanethiol prevents artifactual generation of oxidized DNA bases.

identification of modified DNA bases

by GC/MS
The chromatogram shown in Figure 1A using known
standards is representative of 12 modified DNA bases
monitored in this study. These compounds are: 5-OH-
5MeHyd, 5-OH-Ura, 5-OH-Cyt, 5-OHMe-Ura, cis and
trans Thy Gly, 5,6diOH-Ura, FapyAde, 8-OH-Ade, 2-OH-
Ade, Xan, FapyGua, and 8-OH-Gua. Not included in this
chromatogram are 5-OH-6-H-Thy, which was also
monitored but was not detected in our DNA samples,
and 5-OH-Hyd, a pure sample of which was not
available. However, 5-OH-Hyd (monitored ion 317) was
identified in all of the DNA samples we studied and was
found to elute after 5-OH-5-MeHyd. The internal
standard azaT (monitored ion 256) elutes before 5-OH-5-
MeHyd. Panels B and C of Figure 1 demonstrate typical
chromatograms from PBMCs of a patient immediately
before she received high-dose, infusional doxorubicin.
 Detection of Anabolic Steroid Metabolites in Urine
by GC/MS
A gas chromatography-mass spectrometry (GC-MS) method to determine eight
anabolic steroids (diethylstilbestrol, methyltestosterone, norethindrone, 17α-
ethynylestradiol, estradiol, 6α-methyl-17α-hydroxy-progesterone, estradiol
benzoate, and chlormadinone acetate) was developed..

• Assist. Prof. Dr.. Dhia Falih Al-Fekaiki ©2015

DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS (PAHS) IN
SEAFOOD USING GC-MS: A COLLABORATIVE STUDY

Oil Spill - Gulf Of Mexico 2010

AOAC CALL: PAHS IN FISH AND SEAFOOD

1- Environmental monitoring and cleanup
organic pollutants environmental studies..
2- Criminal forensics
GC-MS can analyze the particles from a human body in order to
help link a criminal to a crime. The analysis of fire debris using
GC-MS is well,.
3- Law enforcement
GC-MS is increasingly used for detection of illegal narcotics,.
4- Sports anti-doping analysis
GC-MS is the main tool used in sports anti-doping laboratories
\anabolic steroids5-Security
6- Chemical warfare agent detection
6- Medicine
metabolic diseases also known.
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