Hybridoma Technology ( Production , Purification , and Application )
PHARMACEUTICAL APPLICATIONS OF GAS CHROMATOGRAPHY(GC), PHARMACEUTICAL ANALYSIS BY P.RAVISANKAR.
1. PHARMACEUTICAL APPLICATIONS OF GAS CHROMATOGRAPHY (GC)
prof. Ravisankar
Vignan Pharmacy college
Valdlamudi
Guntur Dist.
Andhra Pradesh
India.
banuman35@gmail.com
00919059994000
2. High speed: analysis in a matter of
minutes and routine drugs analysis of few
drugs In a matter of few seconds also possible.
High sensitivity we see both rapid analysis as
well as high sensitivity.
For ex is a 2 1/2 min of separation three
common pesticides ,
Methyl parathion,
Malathion,
Ethion at pg levels. Pg means 10-12 grams
these are
parts per billion. This is very good
example of both the high speed as well as a
very sensitive detection.
Applications of gas chromatography:
Gas chromatography (GC) is an instrumental technique used forensically in drug analysis,
arson, toxicology, and the analyses of other organic compounds.
The GC is one of popular instrument used in the world Several (applications)advantages
include
.
3. 2.High resolution: Many compounds can be resolved nicely.
For ex: gasoline has been resolved in to over 300different peaks complex
sample of Petroleum.
Oil refinery – separates fractions of oil for
petroleum products.
13. Gas chromatography – mass spectrometry (GC/MS) is a well established method for
analysis of ignitable liquids.
According to the US Fire Administration, arson is the leading cause of fires and the
second leading cause of deaths and injures, and that’s why arson investigation is of
forensic significance for the criminal justice system.
Commercially available fuels or solvents that are mixtures consisting of hundreds of
components are typically used to start a fire. Analysis becomes very difficult because
ignitable liquids consist of same or similar components at different concentrations, in
addition, fire may evaporate some of the components and thus altering the composition
of residual ignitable liquids found in fire debris.
Analysis, detection, and identification of accelerants in
arson studies are indeed applicable in gas
chromatography.
Novel applications in Gas chromatography:
Arson studies:
Detection of Arson Accelerants Using gas chromatography:
14. For trace evidence, the ability to get the most information from the smallest sample provided, while preserving the maximum
amount for other tests, is critical in delivering results to solve crimes.
Gas chromatography mass spectrometry (GC/MS) is an important technique in the
detection and identification of both bulk drugs and trace level drugs in biological
samples. The PerkinElmer® Clarus® 600 GC/MS is a highly-sensitive and robust system
with flexibility to accommodate the wide range of analyses typical to drug investigations.
Drugs-of-Abuse Analysis by GC/MS
15. Determination of Pesticides, Residue in Aquaculture Products
Detection and Quantitation by Gas Chromatography
Agricultural chemicals such as fertilizers and pesticides have made an important
contribution to agriculture. Pesticides protect crops from pests and diseases.
They have brought about large yield increases. since almost all chemicals that can
kill pests are also potentially damaging to human health. Legislation requires that
pesticide use is appropriately controlled and maximum residue levels (MRLs) not
be exceeded.
Detection method is the process of identifying the pesticides and
determining their concentrations. With the aid of an analytical
instrument, such as a gas chromatograph (GC), we can obtain
information about the original sample by running a standard
solution containing the pesticide(s) at a known concentration and
comparing it with the sample.
16. Description
(±)-Mephobarbital
Hexobarbital
carrier gas: helium, 20 cm/sec @ 275 °C
column: β-DEX 120, 30 m × 0.25
mm I.D., 0.25 μm.
det.: FID, 300 °C
injection: 100:1 split
oven: 210 °C
One enantiomer in the mixture may have an activity or toxicity ... Out of the
many chiral complexing agents used to separate chiral drugs by gas
chromatography (GC).
Barbiturate Enantiomers
application for GC:
18. Blood alcohols (packed application GC)
The determination (accurately measure)of blood alcohol content (BAC) is one of the most
common tests performed by forensic laboratories.
Blood alcohol analysis is used by law enforcement to determine if a driver was unlawfully
operating a vehicle. The results will be used in a court of law, therefore it is important to
minimize systematic and operator errors.
This application note presents the details of an optimized column separation method for
the determination of ethyl alcohol, the internal standard npropyl alcohol, three other
common alcohols, and many potentially interfering common volatiles present in samples
being analysed for measures of driving under the influence of alcohol" (DUI )acronym used
in many regulating districts)
This possible method for determining forensic blood alcohol concentrations.
carrier gas: helium, 20 mL/min.
column: 6 ft. × 2 mm I.D. glass
det.: FID
injection: 1 μL
oven: 85 °C
packing: 5% Carbowax 20M on 60/80 Carbopack B
determination of alcohol (i.e. ethanol) in blood or urine. One obvious application is when
law enforcement agencies need to determine whether or not someone is inebriated. In
these cases, high sensitivity is required since 0.1% blood alcohol content is considered to be
legally intoxicated in most states.
20. Analysis of p-Xylene by GC-FID using a HP-
INNOWax column
The purity of solutions, from relatively pure
solvent such as xylene, to liquors such as
scotch can be also be determined by GC. Two
examples are shown below.
Analysis of Minor Components of Scotch by
GC-FID using a HP-101 Column
22. GC can also be used to
determine the identity of natural
products containing complex
mixtures of similar compounds.
For example, the geographic
source of crude oil or natural gas
can be determined by the
“fingerprint”, or relative
distribution of major and trace
compounds in each oil. Natural
produce oils, such as food
products or fragrances, can be
identified by GC-FID or GC-MS. A
few examples of the separation
of these complex mixtures are
shown below.
23. Common Applications:
Quantification of pollutants in drinking and wastewater
using official U.S. Environmental Protection Agency (EPA)
methods
Quantification of drugs and their metabolites in blood and
urine for both pharmacological and forensic applications
Identification of unknown organic compounds in hazardous
waste dumps
Identification of reaction products
Analysis of industrial products for quality control
ANALYSIS OF VOLATILE ORGANIC COMPOUNDS IN INDOOR AIR
24. Gas chromatography is a physical separation method in where volatile mixtures are
separated. It can be used in many different fields such as pharmaceuticals,
cosmetics and even environmental toxins. Since the samples have to be volatile,
human breathe, blood, saliva and other secretions containing large amounts of
organic volatiles can be easily analyzed using GC. Knowing the amount of which
compound is in a given sample gives a huge advantage in studying the effects of
human health and of the environment as well.
Air samples can be analyzed using GC. Most of the time, air quality control units use
GC coupled with FID in order to determine the components of a given air sample.
Although other detectors are useful as well, FID is the most appropriate because of
its sensitivity and resolution and also because it can detect very small molecules as
well.
GC/MS is also another useful method which can determine the components of a
given mixture using the retention times and the abundance of the samples. This
method be applied to many pharmaceutical applications such as identifying the
amount of chemicals in drugs. Moreover, cosmetic manufacturers also use this
method to effectively measure how much of each chemical is used for their
products.
25. GC and liquid chromatography together just been the primiar techinique for Trace analysis of
organic and inorganic compounds. If I think all the work which is been done in Air polution
and water polutionand food saftery we hv. To analyze pestisides toxic chemicals founds in
Food and food products
we have to analyze the pestiside and food safty and toxic chemicals and food
Porductis and all of these things are daily and rapidly by gc and or liquid chromatographjy.
26. Primary column: Fused silica,30m by.25 mm ID.
5%diphenyl95%dimethyl polysiloxone stationary phase having 0.25 micrometer film thickness.
Secondary column:Fused silica,30m by 0.25mm ID internally coated with a
14%cyanopropyl phenyl and 86% dimethyl polysiloxone stationary phase having .25 µm
Film thickness.
The role of modulator is to collect fractions form chromatographic technique.
It employs 2 columns in series separated by a modulator.
The role of modulator is to collect the fractions from first column( often called as
First dimention column or primary column or 1o column and focus then on to the
Then on to the secondary column or 20 column.
Primany columns tend to be 30m x .25 mm ID.
Secondary columns tend to be 1-2 m X 0.10mm ID are common for secondary columns.
27. Gas Chromatographic Conditions
Gas chromatograph Model: Shimadzu GC-17A, equipped with 63Nielectron capture
detector, attached to a CBM-102 Chromatopak recorder system
Detector: Electron capture detector (ECD)
Column: SPB-608 (Supelco), Capillary (Fused silica), 30m x 0.25mm I. D., 0.25 um
film
Column Oven Temperature: 150o C (4 min) to 290o C at 8o C/min, hold 10 min.
Detector temperature: 300o C
Injector temperature: 220 o C
Carrier gas: Nitrogen (N2) at f low rate of 40 cm/sec.
Measure the area or height of residue peak(s) and determine the residue amount
by comparison to peak area or height obtained from a known amount of
appropriate reference material(s).
28. determination of the VOCs toluene , ethylbenzene ,
o-xylene and cumene (TEXC) in air analysed and quantified using a gas chromatograph
with flame ionisation detection (GC-FID).
Volatile organic compounds (VOCs) are a cause of concern for human health
due to their increased presence in the indoor environment.
They are responsible for a phenomenon known as the sick building syndrome (SBS).
Air monitoring is being used to assess indoor pollution.
29. In most forensic applications of GC, a sample is prepared by dissolving it in a solvent, and the
solution is injected into the instrument using a syringe. For example, to analyze a white
powder suspected of being cocaine, a small portion is weighed out and dissolved in a solvent
such as methylene chloride, methanol, or chloroform. A tiny portion of the sample is then
drawn up into a syringe and injected into the heated injector port of the instrument. The
mobile phase gas (called the carrier gas) also enters the injector port, picking up the
volatilized sample and introducing it into the column where the separation process occurs. If
the sample contains cocaine, it will emerge from the column at a given time (known as the
retention time) that can be compared to the retention time of a known standard sample of
cocaine. The retention time in conjunction with information obtained from the detector is
used to positively identify the compound as cocaine if indeed it is present. Another method
of sample introduction for GC is called pyrolysis, in which a solid sample such as a fiber or
paint chip is heated in a special sample holder to extreme temperatures, causing the sample
to decompose into gaseous components that can then be introduced into the GC. Pyrolysis is
used when the sample is not readily soluble in common GC solvents.
The pharmaceutical industry also heavily uses
GC and HPLC to determine the purity of
reagents, the identity of synthesis products,
and the identity of medicines and illicit drugs.
A few examples are shown below
30. GC-MS used in thyroid cancer study
Gas chromatography-mass spectrometry (GC-MS) has been used to
investigate the pathogenic differences in a form of cancer according to
gender and menopausal condition.
In a study published by BMC(biomed central services publish original
research on oncology)) Cancer, scientists sought to evaluate the
metabolic changes in urinary steroids in men and pre- and post-
menopausal women with papillary thyroid carcinoma (PTC).
GC-MS was used to measure the urinary concentrations of 84 steroids in
all of the patients against corresponding controls.
The metabolic ratio of 2-hydroxy estrone to 2-hydroxy-17 beta-estradiol
in particular showed gender differences in PTC patients.
It is hoped the findings could help better understand the pathogenic
differences in PTC according to gender and menopausal conditions.
31. Separation of m- and p- Xylenes by Gas
Chromatography on Dimethyl
Polysiloxane
short piece of 5% diphenyl 95%
dimethyl column connected to a
wax column.
Cryofocusing was done on the 5
(which still has some diffusivity at -
80°C) and rapid heating to 40°C
restored the wax to a “liquid” to
allow the efficient separation of m-
and p-xylenes. A wax is one of the
only commercially-available capillary
GC stationary phases that will
separate m- and p- xylenes.
32. . One advantages of adsorption( GC) chromatography, as is also true for GSC, is that it is
able to retain and separate some compounds that can not be separated by other
methods. One such application is in the separation of geometrical isomers.
33. Barbiturates are a class of compounds that are central nervous system depressants. They are
categorized as sedatives or hypnotics and are primarily used in the treatment of anxiety,
insomnia, and convulsive disorders. Barbiturates can be analyzed in either
their underivatized or derivatized forms by gas chromatography. Derivatization
of the barbiturates is most commonly performed by methylation of the amido
nitrogens in positions 1 and 3. Methylating reagents like tetramethylammonium
hydroxide (TMAH) and trimethylanilinium anilinium hydroxide (TMPAH) can be used.
Analysis of barbiturates can also be performed on underivatized compounds.
However, underivatized barbiturates have a tendency to produce overloaded
or tailing peaks. Maintain injection port liners, guard columns, and analytical
columns regularly to achieve good peak shape and adequate resolution.
34. Chlordiazepoxide is a long acting benzodiazepine drug. The half-life of Chlordiazepoxide is 5
– 30 hours but has an active benzodiazepine metabolite (desmethyldiazepam) which has a
half-life of 36 – 200 hours.
A rapid gas chromatographic method for the determination of diazepam and metabolites in
body fluids . A rapid method is described for the extraction of diazepam and its metabolites
from plasma and urine. The procedure is applicable to subsequent analysis by electron
capture gas chromatography, and has been used for the analysis of clinical samples. The
detection limit for diazepam is about 0.01 μg/ml,
35. Rapid Method for Determination of Ethanol in Alcoholic
Beverages Using Capillary Gas Chromatography
Ethanol content is very important for the mouth-feel
and flavor of alcoholic beverages. Ethanol contents of
wine, liqueur, and beer range from 7~21%(v/v),
20~50%(v/v), and 3~6%(v/v), respectively
(1). In general,ethanol contents serve as the quality index and taxation
factor for alcoholic beverages(2). After entering WTO,
alcoholic beverages in Taiwan are taxed according to the
ethanol contents, like the taxation system in United
States(3). The higher the ethanol content in an alcoholic
beverage, the higher the tax.
it takes only 7~8 min to complete a
sample analysis for the determination of ethanol content in
a beverage sample. A sample solution (0.5 mL) is mixed
with adequate amount (5 mL) of 1% (w/v) internal standard
solution (acetonitrile, equivalent to 50 mg), and injected
into a capillary GC.
36. Breath Alchohol Testing
Drunk driving costs countless lives and destroys families around the world each year. In
most countries drunk driving is illegal and in pursuing these laws the police utilizes
breathalyzer tests.
Test equipment must be perfectly calibrated to stand up in a court of law. Therefore one
of the calibration methods is to use a calibration gas. The demands on such a calibration
gas are strict, it must be easy to use, be stable, portable and fool-proof. Linde produces
and delivers such calibration gases with the Breathcal program.
Determination of free cholesterol in milk fat:
rapid and direct gas chromatographic (GC) method for determining free cholesterol in
milk fat using a capillary column and programmed-temperature vaporizerinjector was
assayed.
Soil and Water Measurement
Contamination of soil and water can come from many areas, including acid rain,
pesticides industrial waste, landfill, and raw sewage. Analytical procedures include
GC/MS.
37. Environmental measurement is accomplished in many ways. Air samples may be
collected using sample bags or containers and analysed using gas chromatography.
For example, with the US EPA CEMS have a requirement under some environmental
regulations for either continuous compliance determination of the level in which the
facility is out of compliance with acceptable emission standards.
In all areas, a variety of pure gases and calibration gas mixtures are required.
Additionally, due to legal requirements, many of these gas mixtures will need to be
accreditated to international standards.
Air Quality Monitoring
International accords such as the Montreal protocol, or Kyoto accords call on all industry
everywhere to monitor, control and reduce their emissions before discharging them into
the environment. There are a number of different particulate and gaseous emissions
which result from smoke stack emmissions in many industries
including manufacturing, chemical and petrochemical, and power generation.
38. Areas of key measurement include:
Carbon monoxide (CO) from industrial processes and incomplete combustion of wood, oil, gas
and coal.
Carbon dioxide (CO2) , Sulphur Dioxide (SO2), and Nitric oxides (NO and NO2) from
combustion of gas, oil and coal.
Hydrogen sulfide (H2S) and methyl mercaptan (CH3SH) from pulp and paper mills.
Hydrocarbons resulting from incomplete combustion of fuels.
ISO 3930 requirements for vehicle exhaust emission levels for carbon monoxide (CO), carbon
dioxide (CO2), hydrocarbons (HC, in terms of n-hexane), and oxygen (O2).
In all areas, a variety of environmental pure gases and calibration gas standards are required.
Additionally, due to legislative, and/or legal requirements, many of these standards will need
which need manufacturing to accreditation levels.
39. The gas atmosphere must be chosen with due consideration of the particular foodstuff and
its properties. For low-fat products with a high moisture content, it is especially the growth
of micro-organisms that has to be inhibited by using Carbon dioxide. On the other hand,
should the product have a high fat content and low water activity, oxidation protection is
most important and inert Nitrogen would be the preferred choice.
Food packaging
Modified Atmosphere Packaging of food, or MAP, is a natural shelf-life-enhancing method that
is growing rapidly on an international scale. It often complements other techniques, such as
high-pressure and microwave methods or oxygen absorption. The correct gas mixture in MAP
maintains high quality by retaining the original taste, texture and appearance of the foodstuff.
40. Laser Cutting & Welding
Linde technology is being used constantly the world over in laser applications – in
manufacturing, metallurgy, chemicals, food processing, medicine, alternative fuel technologies
& environmental technology. The LASERLINE® concept of high purity gas products and
comprehensive services, applications know-how along with cost efficient gas supply
options forms the basis for customised solutions that maximise productivity
Leak Testing
Producing tight systems is necessary, no matter if you produce tanks for the space shuttle,
automotive gas tanks or gas ditribution systems. Other typical leak test objects are air bags
and pace makers, and anyone can understand what a disaster these could cause if not tight.
Leak testing is often done with a gas or gas mixture together with a "sniffer" which is a
specialized mass spectrometer (MS.) Gas tanks and distribution systems are checked with
helium or helium mixtures while automotive systems often are checked with sulphur
hexafluoride
41. Rapid Analysis of Pesticide Residues in Green Beans:
Pesticide analysis is extremely important due to the need to ensure that foodstuff is not
contaminated with pesticide residues, which can be harmful to human health. Pesticide
analysis poses a number of challenges for laboratories due to the wide ranging chemistries
within the contaminants.
Scientists have used gas chromatography-mass spectrometry (GC-MS) to obtain samples in
order to construct an in-depth human glomerulus proteome database.
They hope the database will help increase the understanding of renal disease pathogenesis,
as well aiding biomarker exploration.
42. Gas chromatography-mass spectrometry used to look at alternative insecticides for control of malaria
Gas chromatography-mass spectrometry has been used to look into
the intesecticidal activity of the essential oils in fruits and seeds taken
from Schinus terebinthifolia Raddiagainst Africa malaria and filarial vectors.
Reported in the Parasites & Vectors journal, research assessed the plant oil against
Anopheles gambiae s.s, An.arabiensis and Culex quinquefasciatus.
The twenty third instar larvae of the
Anopheles gambiaes.s and Cx. quinquefasciatus were exposed to different dosages
of the oil, with mortality rates being observed at 12, 24, 48 and 72 hours.
43. Barbiturates and benzodiazepines are usually encountered by the forensic scientist
as tablet or capsule preparations that have been diverted from licit sources, or,
particularly in the case of barbiturates, as ‘cutting agents’ in other drug materials
(for example, phenobarbitone in heroin samples).
In some cases, identification and confirmation of the dose form can be achieved
by using internationally available databases. If this is not possible, then the
traditional
process of physical description, presumptive testing, TLC and GC–MS
should be followed to identify the drug components. However, some
benzodiazepines
are thermally labile and in such cases HPLC, possibly with diode-array
detection, is often the chosen method of analysis. The latter technique is, in
addition, the preferred method for quantification purposes.
Such drugs, when obtained from licit sources, are very pure and it is therefore
particularly difficult, if not impossible, to compare the samples in order to
determine if they once originated from the same batch.
44. novel method for a rapid measurement of the volatile compounds of food
A fruit juice should not contain ethanol, but in some cases a fermentation can occur. The
maximum ethanol concentration allowed is 0.5% vol. We were asked to propose a rapid
method for the measurement of this ethanol content. The method was as follows: Apple
juice (8ml) was placed in a 22ml vial and ethanol was added in order to obtain a
concentration of between 0.05 and 0.5% vol. The sample was thermostatised at 30°C for
30min. The head-space was sampled using a SPME-fiber, with an adsorption time of 2
min. The desorption took place in the TV9000 in 1 min. The signal was measured with a
FID. The Fig. 5 shows the correlation between the amount of ethanol added and the
area of the signal, for both standard ethanol solutions and spiked samples. The high area
before any addition of ethanol (0 concentration) comes from the volatile compounds of
the apple juice. Using this method, we can determine the concentration of ethanol in
apple juice, and also monitor the evolution of ethanol during the fermentation of apple
juice.
Conclusion
The TV 9000 is...
Simple........
Robust........
Easy to use........
45. Analysis of Anabolic Steroids for Doping Control Purposes by GC
In this application note, the performance of both one dimensional GC-TOFMS and GCxGC-
TOFMS were evaluated, with special attention to the detectability and the confirmation
reliability at low ppb concentration. For this purpose, five anabolic steroids were selected,
for which very low detection limits (2 ng/mL) are required by the World Anti-Doping
Agency.
Qualitative Comparison of Whisky Samples Using Fast GC.
In quality control of alcoholic beverages it is often important to compare different
production batches to detect possible changes in the fermentation and/or distillation
process. This note describes theapplication of a simple and fast GC method with MS
detection using the Pegasus II Timeof-Flight GC/MS detector.
The Application of GC/MS to the Analysis of Pesticides in Foodstuffs
Pesticide contamination of foodstuffs has become a worldwide concern, prompting various
levels of regulation and monitoring.
The discovery of the structure of insulin, for example, was made possible when the British
biochemist, Frederick Sanger, rationally and methodically applied the technique to the
fragments of the ruptured insulin molecule, for which he received the 1958 Nobel prize for
chemistry
46. Because of its simplicity, sensitivity, and effectiveness in separating components of
mixtures, gas chromatography is one of the most important tools in chemistry. It is
widely used for quantitative and qualitative analysis of mixtures, for the purification of
compounds, and for the determination of such thermochemical constants as heats of
solution and vaporization, vapour pressure and activity coefficients. Gas
chromatography is also used to monitor industrial processes automatically: gas streams
are analysed periodically and manual or automatic responses are made to counteract
undesirable variations. Many routine analyses are performed rapidly in environmental
and other fields. For example, many countries have fixed monitor points to
continuously measure the emission levels of for instance nitrogen dioxides, carbon
dioxide and carbon monoxide. Gas chromatography is also useful in the analysis of
pharmaceutical products, alcohol in blood, essential oils and food products.
47. Gas chromatography is widely used for the separation and analysis of mixtures of many
Compounds at very low concentrations .
The compounds which has low boiling points lower than 300oC can be easily analyzed by this
Technique.
The main areas of application of gas chromatography are
1. Analalysis of toxic compounds, solvents, hydrocarbons as well as in forensic field,
2. Polution studies, environmental analysis.
Gas chromatography is mainly used in Pharmaceutical industry for the quantitative as well as
Qualitative estimation of solid, liquid and gaseous organic compounds.
This technique is preferred over spectrophotometry and titration because the separation
As well as (both qualitative and quantitative can be carried out simultaneously.
1.Qualitative analysis:
Identification of the compound by GC either by following ways…
1.Collecting the eluted vapours from the column and subjucting them to specific technique
like Mass spectroscopy,I.R,U.V, NMR etc.
b. The retention time here is used for qualitative analysis. Qualitative analysis
That is to say what is that peak.
The retention time is simply a the time from the point of injection to the peak
Maximum. That is the characteristic of this column and this system these conditions.
48. If the sample under test and the standard compounds are same , then under identical
Conditions their resolution time are also same. Any deviation of graph from the standard
Indicates the presence of a compound other than the standard.
The relative retention R(samle/standard) specific retention volume of sample
= ----------------------------------------------------------------------------
Specific retention volume of standard
2. Quantitative analysis:
The next imp factor is the peak area.
The peak area is used for peak concentration. Twice the concentration twice the peak
Area. This peak area represents the amount of sample which is present in the
Peak. One can also use peak height. The world countries do not have computes
often times simple rulers used for measuring peak heights. But In the modern world
computers and integrates peak areas easily obtained and the results printed out
on the recorders.
49. Pharmaceutical applications : Chromatography plays imp. Role in the analysis of
pharmaceutical products and drugs.
1. Quality control and analysis of drug products and in monitoring metabolites in biological
Fluids.
Antibiotics Penicillins and its derivatives,Gentamycin, kanamycin ,
Neomycin,tetracycline,chloramphenecol.etc.
Anti T.B drugs Ethambutol, Isoniazid, Rifampicin.
Anti cancer drugs 6-mercaptopurin,Flurouracil,Doxorubin,tomoxifen,
Busulfan,Thiotepa,Melfalan.etc.
Antivirals Amantidine,cytarabin,Idoxuridine
CNS stimulants Caffeine, theophylline,Nikethamide
General anaesthetics Chloroform, ether ,ethanol etc.
Sydatives/ hypnotics Barbiturates,Gunathidine, Phenobarbitol (luminol), mephobarbitol,
Benzodiazepens,
Tranquiliazers( some
Major and minor
tranquilizers)
Diazepam(Valium),Chlordiazepoxide (Librium),Flurazepam
(Dalmane),Alprazolam(Xanax),Lorazepam (Ativan),phenothiazine,
identified and measured by GC .etc.
Tri cyclic
Antidepressants and
its
Imipramine,Desipramine,Imitriptyline,Nor triptyline
50. Drug Solid phase Liquid phase Mobile phase Detector
Atropine
sulphate
Acid washed
salinised
Diatomaceous
support.
3% w/w of coated with
phenyl methyl silicone
Fluid.
Nitrogen FID
Homatropine Same as above Same as above Nitrogen FID
Hyoscine
hydrobromidee
yeye drops.
Same as above Same as above Nitogen FID
Clove oil same as above 3% w/w of
PEG.
Nitrogen FID
Ethosuximide
syrup
Same as above 3%w/w of
Cyanopropyl methyl
phenyl,
Silicone fluid.
Nitrogen FID
Steric acid Same as above 15% w/w of
Diethylene
Glycol
Succinate polyster.
Nitrogen FID
51. Ethyl
oestrenol
Glass column acid
washed silanised
diatomaceous
support.
Coated with 3%w/w phenyl
methyl silicone fluid.
Nitorgen FID
Econazole
nitrite cream
same Coated with 3%w/w pf
phenyl methyl silicane fluid
glass column
Nitrogen
FID
Chloroxylenol
solution
Same Coated with 3% PEG
Nitrogen
FID
Fenfluramine
Hcl tablets
Same Coated with 10% PEG and
2% W/W of KOH. Nitrogen
FID
Lincomycin
Hcl
Same Coated with 3%W/W of
phenyl methyl silicone fluid Helium
FID
Mianserin HCl Same Coated with 3% W/W Phenyl
methyl silicone.
Nitrogen FID
Troxidone
caps.
Stainless steel
column packed
with porous
polymer beads
Nitrogen FID
52. 3. Isolation and identification of mixtures of plant extracts, carbohydrates, volatile oils
Amino acids, lipids proteins, preservatives, vitamins, colourants, flavours etc.
4. Identification and determination of fatty acids.
5. Determination of fate of the drugs in body fluids like plasma, serum, urine. Etc.
6.Analysis of solvents, organic functional groups, natural fats ,alcoholic beverages etc.
7. Determination of protective coatings like styrene monomer, vinyl toluene,toluene
diisocyanate etc.
Miscellaneous Applications:
1. Gas chromatography is widely used in the analysis of fertilizers, rubber, cosmetics,
perfumes,food products and petroleum products.
2.For detection of steroids taken by athletes during international sports competitions.
3. IN environmental studies for the isolation and identification of chlorinated pesticids
like DDT and BHC, organomercuric compounds, organophorous compounds,
sulphur compounds etc.
4. For the analysis of dairy products like milk, butter, cheese, etc., for the presence of
aldehyde, ketones, milk sugars and fatty acids. Gas-liquid chromatography is applicable
to species with high critical temperatures and normal boiling points as high as 400° C.
Substances that are solids at normal laboratory conditions
with molecular weights below 1,000 are best separated with liquid-solid or liquid-liquid systems
Lower members of the molecular weight scale range are amenable to
supercritical-fluid separations. Size-exclusion methods are
involved at molecular weights above 1,000. Field-flow fractionation extends
the size range to colloids and microscopic particles.
53. Advantages of combining gas chromatograph and mass spectrograph
There are several advantages of putting the two devices together in one instrument.
For one, it finishes the process faster. The accuracy of both processes is also not
attained when they are done separately. This is because the sample to be taken into
the mass spectrometer must be in its purest state. Once the process is done separately
and the sample is taken out of the gas chromatograph, the sample will be tampered
and the results will differ. Also, when they are done separately, there are instances that
the separated elements in the gas chromatograph have similar ionized fragment
pattern and can be misinterpreted by the mass spectrograph. At least with putting the
two devices together in one instrument, the number of errors is reduced.
54. Environmental checking and cleaning
Have you ever wondered how environmentalists said that our air is already polluted? How did
they come up with such statement? How did they identify the elements that pollute our air?
This is where gas chromatography-mass spectrometry comes in. Supposedly, the air we breathe
should only be composed of O2. Through GC and mass spectrometry, the other elements that
mixed with O2 that make the air polluted are separated and identified each. Through GC and
mass spectrometry, the field of environmental studies has widened.
Criminal Forensics
CSI and NCIS have become the most popular criminal forensic TV series of all times. Have you ever
thought how they are able to solve crimes even without much physical evidences? GC and MS are
responsible for this. When a person is killed with the use of chemical, the chemical as well as the
criminal can be detected through this process. Even without the actual container of the chemical,
it can still be detected through the blood sample of the victim. In arson cases, this is a technique
used to solve the crime, specifically Pyrolysis Gas Chromatography. This is to identify the
elements that caused the fire of the area.
55. Drug identification
Specific drugs are prohibited on every state. In order to detect whether a person is taking
the illegal drugs, GC and MS is applied. Drug test makes use of these processes. Through
this, the examiners can identify what drugs have entered the body of the person through
their urine, blood, and faeces sample.
Security purposes
Since the September 11, 2011 incident, US airports have made their security stricter. To
execute this, all incoming and outgoing individuals of the United States have their baggage
inspected through Thermo Detection. This process involves GCMS to detect whether the
baggage contains explosives.
Analysis of food and beverages for nutrition purposes and perfume
One way to identify the nutrition value of a certain food or drink is through GCMS. Their
elements are identified individually and are then analysed whether they should still be
taken or not.
56. Environmental monitoring and cleanup
GC-MS is becoming the tool of choice for tracking organic pollutants in the
environment. The cost of GC-MS equipment has decreased significantly, and the
reliability has increased at the same time, which has contributed to its increased
adoption in environmental studies. There are some compounds for which GC-MS is not
sufficiently sensitive, including certain pesticides and herbicides, but for most organic
analysis of environmental samples, including many major classes of pesticides, it is very
sensitive and effective.
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 established, and there is even an
established American Society for Testing Materials (ASTM) standard for fire debris
analysis. GCMS/MS is especially useful here as samples often contain very complex
matrices and results, used in court, need to be highly accurate.
57. C-MS is increasingly used for detection of illegal narcotics, and may eventually supplant drug-
sniffing dogs. It is also commonly used in forensic toxicology to find drugs and/or poisons in
biological specimens of suspects, victims, or the deceased.
Security
A post–September 11 development, explosive detection systems have become a part of all
US airports. These systems run on a host of technologies, many of them based on GC-MS.
There are only three manufacturers certified by the FAA to provide these systems,[citation
needed] one of which is Thermo Detection (formerly Thermedics), which produces the EGIS,
a GC-MS-based line of explosives detectors. The other two manufacturers are Barringer
Technologies, now owned by Smith's Detection Systems, and Ion Track Instruments, part of
General Electric Infrastructure Security Systems.
Food, beverage and perfume Analysis
Foods and beverages contain numerous aromatic compounds, some naturally present in the
raw materials and some forming during processing. GC-MS is extensively used for the analysis
of these compounds which include esters, fatty acids, alcohols, aldehydes, terpenes etc. It is
also used to detect and measure contaminants from spoilage or adulteration which may be
harmful and which is often controlled by governmental agencies, for example pesticides.
58. Gas chromatography–mass spectrometry (GC-MS) is a method that combines
the features of gas-liquid chromatography and mass spectrometry to identify
different substances within a test sample. Applications of GC-MS include drug
detection, fire investigation, environmental analysis, explosives investigation,
and identification of unknown samples. GC-MS can also be used in airport
security to detect substances in luggage or on human beings. Additionally, it
can identify trace elements in materials that were previously thought to have
disintegrated beyond identification.
GC-MS has been widely heralded as a "gold standard" for forensic substance
identification because it is used to perform a specific test. A specific test
positively identifies the actual presence of a particular substance in a given
sample. A non-specific test merely indicates that a substance falls into a
category of substances. Although a non-specific test could statistically suggest
the identity of the substance, this could lead to false positive identification.
59. From war zones or scenes of natural disasters, news reporters often comment on the
stench of decaying bodies. This characteristic malodour is made up of a complex mixture
of volatile compounds that might be useful in forensic pathology, to establish the cause
of death and the post-mortem interval. In the normal world, this characteristic smell is
also well known to members of the police force, crime scene technicians, medical staff
and forensic pathologists, as well as to some dogs. Its composition is the trigger used by
tracker dogs to locate hidden bodies. The same odour is also recognised by insects that
quickly colonise a body once it begins to decay. Now, Greek researchers have suggested
that the odour can be used to determine the time since death and possibly help to
establish the cause of death. First of all, they remind us that the VOCs that constitute the
smell arise from the same sources in each human corpse. Carbohydrates in the body
break down to give mainly oxygenated compounds (alcohols, aldehydes, ketones, acids,
esters, ethers), proteins degrade to nitrogen, phosphorus and sulphur compounds,
nucleic acids from nitrogen and phosphorus compounds and lipids decompose to
nitrogen, phosphorus and oxygenated compounds and hydrocarbons. So, in theory,
different decaying bodies should produce the same set of VOCs.(volatile organic
compounds) he adsorbed gases were analysed by thermal desorption GC/MS and the
components were identified from their retention times and mass spectra using a
commercial database and an in-house database constructed from standard compounds.
The results were described in Forensic Sci. Intl. 2005. A total of 86 substances were
identified and quantified with the aid of internal standard compounds. he relatively high
levels of toluene were unexpected, leading the authors to hint at the possibility of toluene
poisoning of the victims. The high number of fatty acid esters found was explained in
GC and the smell of death(corpses)