• Title/Summary/Keyword: GC-MS/MS

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Chiral Derivatization of Hydroxycarboxylic Acids Using 2,4,6-Trichlorobenzoyl Chloride as a Highly Efficient Regioselective Esterification Reagent for Gas Chromatography-Mass Spectrometry

  • Park, Jeong Hyeok;Han, Sang Yun
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.103-107
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    • 2020
  • We report the application of 2,4,6-trichlorobenzoyl chloride (often referred to as Yamaguchi esterification reagent) for the selective derivatization of the carboxylic group for GC-MS with the sample preparation method optimized for GC-MS analysis. The reagent was shown to be capable of selectively turning the carboxylic group into a reaction center, i.e., anhydride, of which the further reaction was directed to a near complete formation of required esters by unique steric and electronic effects of the reagent. Using the developed method, the chiral separation of hydroxycarboxylic acids by GC-MS using non-chiral columns was successfully demonstrated.

A Low-Cost Open-Source Air Sampler for the Sorbent Tube Sampling for TD-GC/MS Analysis

  • Jang, Hwa-yong;Oh, Han Bin
    • Mass Spectrometry Letters
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    • v.11 no.4
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    • pp.95-102
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    • 2020
  • In this study, we provide full descriptions of how to make a low-cost and completely open-source laboratory-made air sampler that will be used for sample adsorption for thermal desorption-gas chromatography mass spectrometry (TD-GC/MS) analysis. It is well known that harmful gases cause bad effects on human bodies, so it is necessary to identify the types and amounts of gases in industrial sites. One of the most commonly used methods for gas sampling is to utilize a sorbent tube using an air sampler. Commercially available air samplers are expensive, typically priced between $1,000 and $2,000, and their design often cannot be modified to fit the experiment. To address these shortcomings, we have developed a do-it-yourself (DIY) air sampler that is not only cheap enough, but also completely open-source. Furthermore, the performance of the fabricated air sampler was validated in conjunction with TD-GC/MS for the analysis of volatile compounds.

Fundamental study on the development of the testing method of Triclosan with GC/ECD and GC/MS (GC/ECD 및 GC/MS를 이용한 트리클로산 정량분석에 관한 기초 연구)

  • Jeong, Hui-Jae;Lee, Jae-In;Kweon, Deok-Jun;Eom, Hui-Jeong;Choi, Zel-Ho;Choi, Ki-In
    • Analytical Science and Technology
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    • v.25 no.6
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    • pp.410-415
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    • 2012
  • In this study, a fundamental study was conducted to establish the method for quantitative analysis and pretreatment of triclosan, one of the chemicals to be used as bactericides, detergents, and sterilizers. The extraction efficiency of triclosan was the highest when it was extracted by soxhlet apparatus with n-hexane, and it showed a satisfactory result when the samples were analyzed with both GC/ECD and GC/MS. To evaluate the reproductivity of the results, each 30 reference samples made with paper filter and cotton wool was prepared in this study. From the results with high extraction effectiveness, low analysis deviation, and good statistical analysis data, the method for the extraction and analysis for triclosan were resonable for the paper and textile samples applied in this study.

The Stimultaneous Determination of Phenolic Compounds by GC and GC/MS

  • Kim, Jong-Bae;Park, Jyung-Rewng
    • Preventive Nutrition and Food Science
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    • v.3 no.2
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    • pp.111-118
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    • 1998
  • To develop a simple, rapid and simultaneous analytical method of phenolic compounds using gas chromatography (GC) and gas chromatography/mass spectrophometer (GC/Ms), this experiment was carried out to search the retention times of capillary columns and the characteristics of fragment ions in electron impact mass spectra. Most of trimethylsilyl derivatives and underivatized phenolic compounds were separated very well on three kinds of capillary columns(HP-1), Ultra-2 and HP-35). Quantitiative determination of phenolic compounds was achieved by internal standards (p-hydroxybenzoic acid iopropyl ester, p-hydroxybenzoic acid ethyl ester). Calibration plts were linear in the investigated range, and the limits of detection were about 5 ng at split mode method. When analyzed by three columns, theseparation times were fairly constant on two nonpolar columns, but a few compounds showed slightly different separation order by the itnermediate polar HP-35 column. The important characteristic patterns of TMS derivatives of phenolic compounds on the EI/MS spectrra appeared at the base peak of [M-15]+ ion and presented at high abundance in most TMS derivatives of phenoloc compounds. [M]+, [M-CH3-COO]+, [M-Si(CH3)4]+ and [M-Si(CH3)4 -CH3]+ also observed in mass spectra of these compounds . Although several compounds have the same retention times on GC column, it might be possible to identify these compounds by the different patternsof mass frgement ions. The TMS derivatives, thus , provide additional information for identification of phenolic compounds in biological systems.

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Analysis of UV Filters in Water using Stir Bar Sorptive Extraction (SBSE) and GC/MS-MS (교반막대 추출법과 GC/MS-MS를 이용한 수중의 자외선 차단제 분석)

  • Seo, Chang-Dong;Son, Hee-Jong;Jung, Jong-Moon;Choi, Jin-Taek;Jang, Seong-Ho
    • Journal of Environmental Science International
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    • v.23 no.6
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    • pp.1037-1047
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    • 2014
  • A highly sensitive analytical method based on stir bar sorptive extraction (SBSE) technique and gas chromatography/tandem mass spectrometry (GC/MS-MS) has been developed, allowing the simultaneous multi-analyte determination of seven UV filters in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 40 mL of water sample at pH 3 and stirred at 1,100 rpm for 120 min. Other SBSE parameters (salt effect and presence of organic solvent) were optimised. The method shows good linearity (coefficients > 0.990) and reproducibility (RSD < 12.9%). The extraction efficiencies were above 84% for all the compounds. The limits of detections (LOD) and limits of quantification (LOQ) were 2.1~8.6 ng/L and 6.8~27.5 ng/L, respectively. The developed method offers the ability to detect 8 UV filters at ultra-low concentration levels with only 40 mL of sample volume. Matrix effects in tap water, river water, wastewater treatment plant (WWTP) final effluent water and seawater were investigated and it was shown that the method is suitable for the analysis of trace level of 7 UV filters except of benzophenone (BP). The method developed in the present study has the advantage of being rapid, simple, high-sensitive and both user and environmentally friendly.

Partial Reduction of Dinitroaniline Herbicide Pendimethalin by Bacillus sp. MS202 (Bacillus sp. MS202에 의한 Dinitroaniline계 제초제인 Pendimethalin의 부분환원)

  • Lee, Young-Keun;Chang, Hwa-Hyoung;Jang, Yu-Sin;Hyung, Seok-Won;Chung, Hye-Young
    • Korean Journal of Environmental Agriculture
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    • v.23 no.4
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    • pp.197-202
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    • 2004
  • The persistence of pendimethalin in soil and ground water has an injurious effect on ecosystem. Pendimethalin-degrading bacterium was isolated from Masan, Gyeongnam province and temporarily identified as Bacillus sp. MS202 by the analysis of API CHB50, kit, FAME, and 16S rDNA sequence. from the analysis of pnedimethalin metabolite using TLC, GC, and GC-MS, we found that the degradation of pendimethalin by Bacillus sp. MS202 did not result in the dealkylated form, but the formation of the reduced compound, 6-amino-2-nitro-N(1-ethylpropyl)-3,4-xylidine or 2- amino-6-nitro-N(1-ethylpropyl)-3,4-xylidine.

A Study on Experimental Characteristics in Fire Investigation Techniques of Flammable Liquids (유류화재의 감식기법의 실험적 특성에 관한 연구)

  • Hwang, Taeyeon;Choi, Donmook
    • Fire Science and Engineering
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    • v.26 no.6
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    • pp.7-14
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    • 2012
  • This paper is to develop analytical techniques of flammable liquids which have been used for accelerating fire in accidental fires and arsons. We tested the temperature distribution of ceiling, fire patterns on the floor, and existence of flammable liquids and a check with GC/MS about flammable liquids comparing with papers, newspapers, and clothing. Research findings are as follows. The temperature of ceiling is influenced by flame. So gasoline and thinner was observed that combustible materials would be burned by flame. The fire patten on the floor was observed that flammable liquids had specialized pattern comparing combustible materials. When combustible materials on the PVC (Polyvinyl chloride) floor was burned, they didn't react to the gas detector. But flammable liquids had opposite results. After 7 days, we identified components of fire residues with the GC/MS (Gas Chromatography/Mass Spectrometry) about existence of flammable liquids and got components of flammable liquids. Fire investigation is a complicated processes. But we understand characteristics of materials, need detail investigations, and use the GC/MS to analyse flammable materials.