Application Of Capillary Gas Chromatography Research Articles

METHODICAL SUPPORT FOR CONTROL OVER THE CONCENTRATION OF PERSISTENT ORGANIC POLLUTANT HEXACHLOROBENZENE IN BLOOD

Introduction. Persistent organic pollutants (POP) are extremely dangerous compounds contaminating the environment and exerting the negative impact on human health. Organochlorine pesticides, including hexachlorobenzene, are a specific group among POP. Our research goal is methodological support for the hexachlorobenzene content control in human biological environments. Material and methods. We developed highly both sensitive and selective procedure for determining hexachlorobenzene in blood. Hexachlorobenzene determination in blood is based on the application of capillary gas chromatography with linear programming of a column temperature, electron capture detector (ECD), and extraction with an organic solvent at a sample preparation stage. When implementing the developed methodology, the following indices were evaluated: accuracy and error characteristics of the analysis results. The lower limit of hexachlorobenzene quantification (LOQ) in blood amounted to 0.000024 µg/cm3, with the range of detectable concentrations from 0.00015 to 0.005 (determination method error ≥ 20%), which allows to adequately diagnose chemical burden with a highly toxic persistent organic pollutant in blood. Results. The results of quantitative chemical analysis of hexachlorobenzene contents in blood had the following quality indices: precision and correctness amounted to 15.621%; repeatability - 3.45%; reproducibility - 4.65%. In the process of testing the method, concentrations of hexachlorobenzene in the range of 0.0003 ± 0.0001 ÷ 0.0007 ± 0.0001 μg/cm3 were detected in the blood of the examined group. Discussion. The high efficiency of gas chromatography determination of hexachlorobenzene in blood was achieved via selection of optimal conditions for chromatographic analysis: capillary column HP-1- 35m∙0.32mm∙0.25µm with linear programming of column temperature, carrier gas (nitrogen), electron capture detector (ECD). The developed method of the preparing a blood sample for analysis, including liquid extraction with toluene, protein denaturation by centrifuging the biological medium at 7000 rpm for 15 min at pH of 6-7 in combination with gas chromatographic analysis and an electron capture detector (ECD) made it possible to complete extraction of hexachlorobenzene from blood in an amount of 99.7%.

Хроматографические методы в анализе и идентификации виноградных вин

The analysis of the published works, standard documents and the original articles devoted to the methods of the analysis of wines was carried out. It was shown that during the analysis of wine materials for the practical and scientific purposes, the chromatography methods, which allow determining a wide range of the core organic and mineral substances and also traces of other components, were used most often. On the basis of the literature data analysis, the assessment was made of the basic components’ contents in wines of various geographical origins with the use of several chromatography methods. The analytical aspects of studying the composition and the prospective factors complicating the interpretation of the analysis results were discussed. Specific features and applications of the various options of a high performance liquid chromatography method were examined for assessing the quality of wine production. Questions of the application of capillary gas chromatography, gas and tandem mass spectrometries for the determination of the components of grape wine were considered. Publications and the developed procedures of the quality assurance of the wines realized with the application of capillary electrophoresis methods were discussed in additional detail. The limits of components detection, errors, compositions of electrolytes, and the basic conditions of the analysis were presented. (Russian) Keywords : organic and nonorganic components of wine, gas chromatography, high performance liquid chromatography , capillary electrophoresis DOI: http://dx.doi.org/10.15826/analitika.2015.19.4.013 Yu.F. Yakuba 1 , Z.A. Temerdashev 2 1 North Caucasian Regional Research Institute of Horticulture and Viticulture , Krasnodar, Russian Federation 2 Kuban State University, Krasnodar, Russian Federation

Ultra-short open capillary columns in gas–liquid chromatography

New area in capillary gas chromatography (GC) was investigated. Many important analytical tasks can be solved only use very short capillary columns. Variation of chromatographic characteristics of ultra-short capillary columns with column length was originally studied at the conditions of gas–liquid chromatography. The column length varied from 500 to 10 cm. Dependencies of height equivalent to one theoretical plate (HETP) and separation number (SN) on carrier gas velocity were considered for columns of various length. Field of ultra-short open capillary columns in gas–liquid chromatography has the following peculiarities: (1) more shorter retention times of sorbates, (2) more low temperatures of short column, that has as final result (a) high selectivities of used column and (b) the possibilities to separation more thermal lability compounds. It was shown that short capillary columns can be successfully used at both isothermal and temperature programming conditions for express-analysis at lower oven temperatures. Examples of express-analysis (high speed), analysis of high boiling and thermolabile compounds are listed, which demonstrate some radically new applications of capillary gas chromatography.

Application of capillary gas chromatography to the determination of ethylene glycol migration from PET bottles in Brazil

Application of capillary gas chromatography to the determination of ethylene glycol migration from PET bottles in Brazil

Application of capillary gas chromatography to the study of hydrolysis of the nerve agent VX in rat plasma.

We present here a gas chromatography technique allowing the detection and quantification of VX [O-ethyl S-(2-diisopropylaminoethyl)methylphosphonothiolate] as well as its P-S bond hydrolysis product diisopropylaminoethanethiol directly from spiked rat plasma. This technique was applied to study VX hydrolysis in rat plasma. We observed that 53 +/- 4% of 374 microM VX disappeared from spiked plasma after 2 h. VX disappearance was mainly related to enzymatic cleavage of the P-S bond (Km = 2.5 mM and Vmax = 13.3 nmol min-1 ml-1 of rat plasma). The activity was totally inhibited by 1 mM Hg2+ and was also inhibited by metal chelators.

Environmental applications of capillary gas chromatography coupled with atomic emission detection — a review

AbstractEnvironmental applications of capillary gas chromatography coupled with atomic emission derection (GC‐AED) have been reviewed with emphasis on both the commercial and laboratory‐built systems. Attention was focused on (1) element‐selective detection of non‐metallic as well as metallic pollutants, (2) identification of contaminants, and (3) sample preparation considerations.

Ultra-trace Analysis of Metosulam, a New Triazolopyrimidine Herbicide, in Soil Using LC-UV and TSP-LC-MS

Abstract Metosulam (DE-511), N-(2,6-dichloro-m-tolyl)-5,7-dimethoxy-[1,2,4] triazolo [1,5a]pynmidine-2-sulphonamide is a new selective herbicide developed for the control of broadleaf weeds in cereals and maize. The application of new generation low use rate herbicides, such as metosulam, has in turn created the need for the development of ultra-trace residue methodologies. To help investigate the environmental impact of metosulam, levels at sub-part per billion (μg/kg) in soil were determined. Application of capillary gas chromatography, with various injector systems, was unable to analyse metosulam methyl derivative due to the inherent thermal instability of the molecule. Liquid chromatography with ultraviolet detection (LC-UV) was used to quantify residues of the herbicide following a series of selective clean-up procedures. The chosen methodology used simple reagents plus standard equipment and although the molar absorbtivity of metosulam is poor, analysis of soils of various texture classes at the desired sensitivity level, was achieved. Thermospray Liquid chromatography with mass spectrometry (TSP-LC-MS) was used as a confirmatory technique for the analysis of metosulam in the same soils. Excellent agreement between the two techniques was observed. Details of the clean-up procedures used to produce desired selectivity and the relative merit of the two detection systems are discussed.

The stereochemistry of commercial 2,6-dimethylcyclohexanone: An application of capillary gas chromatography

ADVERTISEMENT RETURN TO ISSUEPREVLab-ExptNEXTThe stereochemistry of commercial 2,6-dimethylcyclohexanone: An application of capillary gas chromatographyCharles M. Garner Cite this: J. Chem. Educ. 1993, 70, 12, A310Publication Date (Print):December 1, 1993Publication History Received3 August 2009Published online1 December 1993Published inissue 1 December 1993https://doi.org/10.1021/ed070pA310RIGHTS & PERMISSIONSArticle Views488Altmetric-Citations1LEARN ABOUT THESE METRICSArticle Views are the COUNTER-compliant sum of full text article downloads since November 2008 (both PDF and HTML) across all institutions and individuals. These metrics are regularly updated to reflect usage leading up to the last few days.Citations are the number of other articles citing this article, calculated by Crossref and updated daily. Find more information about Crossref citation counts.The Altmetric Attention Score is a quantitative measure of the attention that a research article has received online. Clicking on the donut icon will load a page at altmetric.com with additional details about the score and the social media presence for the given article. Find more information on the Altmetric Attention Score and how the score is calculated. Share Add toView InAdd Full Text with ReferenceAdd Description ExportRISCitationCitation and abstractCitation and referencesMore Options Share onFacebookTwitterWechatLinked InReddit PDF (1 MB) Get e-Alerts Get e-Alerts

Applications of capillary gas chromatography to the quality control of butter and related products

Analyses performed to establish the quality of butter are essentially based on the packed column gas chromatographic determination of fatty acid composition. One of the main problems is the determination of the short-chain fatty acids, particularly butyric acid. In previous work, comparing results obtained by on column injection with those obtained by split injection, with and without silanized glass-wool in the liner, at two different pre-set splitting ratios, it was found that a packed injector at the highest splitting ratio gives results equivalent to those obtained with on-column injection. When small amounts of butyric acid must be detected, less volatile esters are more suitable than those obtained by rapid transesterification with sodium butoxide. In this paper results obtained for the determination of the amount of butter in bakery products are reported. Results for both real samples and model systems gave highly significant values for the correlation coefficient for split and on-column injection on the basis of fatty acid butyl esters. Triglycerides were also determined in order to measure the amount of butter by means of trienanthine.

Application of capillary gas chromatography to a survey of wheat for five trichothecenes.

A previously published method for the determination of deoxynivalenol (DON) and nivalenol (NIV) in grains by capillary gas chromatography (GC) with electron-capture detection (ECD) has been modified to include HT-2 toxin (HT-2), T-2 toxin (T-2) and diacetoxyscirpenol (DAS). Recoveries of the five trichothecenes from wheat averaged 71-92% in the range 0.8-4 micrograms/g. Detection or quantitation limits found in two laboratories were from 0.02 to 0.4 micrograms/g, with those for T-2 and DAS at the high end of this range. The method proved of practical use in survey work for the screening and determination of these trichothecenes in wheat from the 1987 western Canadian crop. There were no false positives for HT-2, T-2 and DON in durum and HY-320 wheat. However, interferences precluded the determination of 4- and 15-monoacetoxyscirpenol (MAS) by GC-ECD. The natural occurrence of HT-2 toxin (0.06-0.59 micrograms/g) was demonstrated by GC-ECD and confirmed by GC-mass spectrometry (MS) in 23 samples of durum and HY-320 wheats (1986 and 1987 crops); it was almost always accompanied by DON and in one sample a low concentration of NIV (0-05 micrograms/g). False positives for HT-2 and DAS in red spring wheat detected in 1987 by GC-ECD were 6% (nearly all identified as variety Katepwa) and 8%, respectively. Hence confirmation of suspected HT-2 and DAS by GC-MS is necessary, particularly with red spring wheat.

Some applications of capillary gas chromatography in clinical chemistry

AbstractProfile analysis using capillary gas chromatography is applied in clinical chemistry to detect metabolic abnormalities. Examples are the increase of the urinary excretion of aromatic acids carrying a 4‐hydroxyl group and the decrease of hippuric acid in liver cirrhosis, and the elevated concentrations and excretions of dicarboxylic, oxocarboxylic, and hydroxycarboxylic acids in diabetes mellitus. Gas chromatographic quantitations, in some instances using mass selective detection, are performed on clinically relevant constituents. An example is the investigation of plasma and urinary hippuric acid and 3‐carboxy‐4‐methyl‐5‐pro‐pyl‐2‐furanpropionic acid in different stages of renal diseases.

Application of capillary gas chromatography with mass selective detection to pesticide residue analysis

A random sample of 76 pesticides with good gas chromatographic properties has been collected in order to test the applicability of the mass selective detector HP MSD for pesticide residue analysis. Using a capillary column, mass spectra of good quality were produced with 10 or 20 ng of each pesticide. Seventy two compounds were not only identified at this concentration with the PBM (probability based matching) search routine in the NBS library, but also remarkably with the best fit in the corresponding hit list. Lower concentrations can be detected only with selected ion monitoring (SIM). A mixture of 18 chlorinated pesticides was added to green pepper at the 10 ppb level. All compounds were detected with SIM using special time programming in one gas chromatogaphic analysis. The detection sensitivity of the mass selective detector in SIM mode approaches that of established selective detectors. The reliability of the results with respect to the identity of a pesticide residue, however, is orders of magnitude better. Therefore, this detector is a valuable tool for performing confirmatory analysis.

Application of capillary gas chromatography to environmental analysis

AbstractRoutine analytical methods for benzo[a]pyrene and nitroarenes in airborne particulates are presented. Benzo[a]pyrene in airborne particulates was easily analyzed by a capillary GC/NCIMS. Analysis time was about 10 min and analytical values obtained by this method agreed well with those by HPLC/spectrofluorometry. Nineteen nitroarenes were analyzed by capillary GC/FTD following a simple clean‐up procedure. Fifteen out of 19 nitroarenes analyzed were mutagenic for Salmonella typhimurium TA100 and TA98, and 4 nitroarenes were carcinogenic to experimental animals.

Application of capillary gas chromatography for physico-chemical measurements particularly considering the influence of adsorption on the liquid phase-tube wall interface

Utilization of capillary chromatography for the quantitative definition of the thermodynamic values of the solute/liquid phase interaction is shown. A method is given to define the pure values of the distribution coefficients of volatile compounds in a gas-liquid phase system with the use of an intermediate standard for which adsorption interaction can be neglected. It is shown that the definition of the heats of solution of polar solutes in a cross-linked liquid phase leads to higher values if adsorption interaction is not taken into account.

Some applications of capillary gas chromatography in the chemical industry

AbstractAbout three years ago, fused silica capillary columns were introduced in the Quality Control Laboratory of the Shell refinery/chemical complex at Pernis. In general, long, thick‐film, wide‐bore capillary columns are used together with low split ratios and hydrogen as carrier gas. These conditions enable the analysis of relatively large sample amounts, resulting in low detection limits for the minor components without overloading by the major components, while still maintaining a satisfactory resolution. A number of applications are shown, such as the analysis of complex mixtures, the determination of trace impurities and the analysis of residual volatiles in polymers.

Application of capillary gas chromatography with electron capture detection and split‐splitless injection to the evaluation of volatile halogenated hydrocarbon removal using hydrogen peroxide after break‐point chlorination in drinking water treatment

AbstractIn this paper we report a way to evaluate the removal of volatile halogenated hydrocarbons formed after break‐point chlorination in the Arno river raw water at the Mantignano Utility, Florence, Italy, following dechlorination by hydrogen peroxide. The removal evaluation is performed by GC‐ECD on fused silica capillary columns with split‐splitless injection on n‐pentane extracts and by other analytical techniques such as UV254 absorption, TOC and TOX. Both laboratory and pilot plant data on Arno river raw water are reported and discussed.

Application of capillary gas chromatography in the stability control of phthalate-ester-type poly(vinyl chloride) plasticisers treated with light and plasma

By means of high-resolution capillary gas chromatography we followed the change in composition of poly(vinyl chloride) plasticisers during treatment with light of a wide range of wavelengths and with plasma. The composition is not significantly altered by either treatment, therefore the plasticisers would not appear to be respon sible for the ageing of soft poly(vinyl chloride).

The Application of Capillary Gas Chromatography to the Analyses of Acidic Constituents of Tobacco Leaf and Smoke

Abstract Extensive details are presented for the laboratory preparation of specific glass capillary columns for the gas chromatographic analysis of various phenolic and acidic compounds of leaf and smoke. The chromatography of derivatized and underivatized mono- and dihydroxybenzenes, volatile acids, phenolic acids, and fatty acids is evaluated on both Pyrex glass and fused silica columns prepared by our methodology. The stability, efficiency, and low surface activity of columns prepared from different liquid stationary phases (SE-54, Superox-4, SP-1000, Silar 10C) are illustrated by numerous separations.

Potential of capillary gas chromatography in industrial research laboratories

The pros and cons of the application of capillary gas chromatography in an industrial research laboratory are discussed. The consequences of using a capillary instead of a packed column are dealt with, especially with respect to the injection technique and detection. Examples of separations in the fields of product evaluation and trace analyses are discussed.

Retention Time Data for Organochlorine, Organophosphorus, and Organonitrogen Pesticides on SE-30 Capillary Column and Application of Capillary Gas Chromatography to Pesticide Residue Analysis

Abstract Relative retention time data for 194 pesticides and metabolites are reported for a 15 m SE-30 capillary gas chromatographic column under a single temperature programmed regime. The reproducibility of retention time and quantitation is discussed and the performance of electron capture and nitrogenphosphorus thermionic detectors is evaluated in relation to pesticide residue analysis.