Non-isothermal pyrolysis property analysis of biomass using pyrolyzer-gas chromatography/mass spectrometry

신강호,최예진,김영민 한국공업화학회 2020 한국공업화학회 연구논문 초록집 Vol.2020 No.-

Pyrolyzer-gas chromatography is an useful investigation tool for the pyrolysis kinetic properties and its product analysis of biomass. Recently, various kinds of analytical methods, such as evolved gas analysis-mass spectrometry and multi-shot pyrolysis-gas chromatography/ mass spectrometry, were effectively applied to understand the pyrolysis behavior of biomass. In this study, evolved gas analysis-mass spectrometry and multi-shot pyrolysis-gas chromatography/mass spectrometry of pine nut shell was performed to provide the non-isothermal reaction properties and understand its reaction mechanism.

Gas Chromatography/Mass Spectrometry를 이용한 팔강약침액 성분에 대한 연구

김협,안병수,Kim, Hyub,Ahn, Byung-Soo 대한약침학회 2008 Journal of pharmacopuncture Vol.11 No.3

Objective: The purpose of this study was to investigate the composition for pharmacopunctures of eight principles hydrodistillation layer. Methods: The study was determined the hydrodistillation layer for pharmacopunctures of eight principles by hydrodistillation method. The effective components in hydrodistillation layer for pharmacopunctures of eight principles were extracted with ethyl ether or dichloromethane, and then analyzed by Gas Chromatography/Mass Spectrometry(GC/MS). Results: 1. Analyzed pharmacopunctures of eight principles by GC/MS, a lot of differences according to extraction solvent by each pharmacopunctures of eight principles and specific peak patterns were seen. 2. The main compound in pharmacopunctures of eight principles was a kind of hexaoxacyclohydrocarbon that has long hydrocarbon chain.

Effect of Stewing Time on the Small Molecular Metabolites, Free Fatty Acids, and Volatile Flavor Compounds in Chicken Broth

Rong Jia,Yucai Yang,Guozhou Liao,Yuan Yang,Dahai Gu,Guiying Wang 한국축산식품학회 2024 한국축산식품학회지 Vol.44 No.3

Chicken broth has a taste of umami, and the stewing time has an important effect on the quality of chicken broth, but there are fewer studies on the control of the stewing time. Based on this, the study was conducted to analyze the effects of different stewing times on the sensory, small molecular metabolites, free fatty acids, and volatile flavor compounds contents in chicken broths by liquid chromatography-quadrupole/timeof- flight mass spectrometry, gas chromatography-mass spectrometry, headspace solidphase microextraction, and gas chromatography-mass spectrometry. Eighty-nine small molecular metabolites, 15 free fatty acids, and 86 volatile flavor compounds were detected. Palmitic and stearic acids were the more abundant fatty acids, and aldehydes were the main volatile flavor compounds. The study found that chicken broth had the best sensory evaluation, the highest content of taste components, and the richest content of volatile flavor components when the stewing time was 2.5 h. This study investigated the effect of stewing time on the quality of chicken broth to provide scientific and theoretical guidance for developing and utilizing local chicken.

Determination of Persistent Organochlorine Pollutants in Rat Hair by Gas Chromatography-Mass Spectrometry

Ho-Sang Shin*,Heesoo Pyo,Song-Ja Park 대한화학회 2004 Bulletin of the Korean Chemical Society Vol.25 No.10

A gas chromatography/mass spectrometric assay method was developed for the determination of persistent organochlorine pollutants (POPs) in hair. For the exact extraction study was used hair of rat exposed with POPs. Sonication of the hair matrix with 3 M HCl solution in methylene chloride of the extraction methods studied was the most efficient and rapid sample preparation method. After sonication of rat hair was achieved clean up with a solid phase extraction procedure using silica gel-florisil. Elution was performed with 8 mL of methylene chloride. The eluate was concentrated to approximately 100 L and analyzed by gas chromatography-mass spectrometry (GC-MS). Detection limits of POPs were in the concentration range of 0.6-1.2 ng/g in rat hair. Aldrin, dieldrin, p,p-DDT and mirex were dosed rat for 4 weeks at concentration of 0.01mg/L in drinking water and detected in rat hair at concentration of 2.8, 11.3, 7.9 and 15.6 ng/g, respectively. Aldrin and p,p-DDT were metabolized to dieldrin and p,p-DDE, which were detected in concentration of 9.7 and 2.9 ng/g in rat hair, respectively. The developed method may be valuable to be used to analyze POPs in human hair.

Determination and quantification of arbutin in plants using stable isotope dilution liquid chromatography–mass spectrometry

김태진,박영진,박상언,하선화,김재광 한국응용생명화학회 2018 Applied Biological Chemistry (Appl Biol Chem) Vol.61 No.5

Arbutin is a very safe whitening agent for human skin. Since it is more expensive than other agents and has a challenging synthesis, novel methods to obtain this valuable agent are needed. In this study, we developed a precise and accurate method to detect and quantify arbutin using stable isotope dilution liquid chromatography–mass spectrometry (LC–MS). One challenge that needed to be overcome was the matrix effect occurring during the LC– MS analysis due to the analyte ionisation enhancement or suppression in the electrospray ionisation source by coeluting compounds. Notably, arbutin had different matrix effects in the various sample matrices. A solution to this problem was the use of [d4]-arbutin as a stable isotopelabelled internal standard (SIL-IS), as it compensated the matrix effect of arbutin because it was affected by almost the same matrix effect. The validation of the developed method showed excellent linearity (r2 = 1.000), precision (relative standard deviation B 2.5%), accuracy (recovery, 97.42–98.52%), limit of detection (0.03 lg/mL), and limit of quantification (0.1 lg/mL). Finally, the method of arbutin detection was applied to blueberry leaves to compare the precision and accuracy results obtained by performing stable isotope dilution using LC–MS and gas chromatography–mass spectrometry. The method was applied to strawberry leaves and pear peels, indicating that the SIL-IS method can be expected to find application in the arbutin analysis in other plants.

기체크로마토그래피/ 질량분석기를 이용한 인체 내 뇨시료에서의 Tamoxifen 대사체 검출을 위한 유도체화 연구

김연제,이윤정 한국분석과학회 2004 분석과학 Vol.17 No.4

The improved derivatization technique of tamoxifen metabolite in human urine is described for the acylation method that they are substituted by derivatization reagent like acyl anhydride for use of gas chromatography/mass spectrometry. The hydroxyl group of tamoxifen metabolite was derivatized by trifluoroacetic anhydride(TFAA), pentafluoroacetic anhydride(PFPA) and heptaflorobutylic anhydride (HFBA). It was investigated to the gas chromatography/mass spectrometry(GC/MS) technique use negative ion chemical ionization(NCI), positive ion chemical ionization(PCI) and electron impact(EI). In acylation of the metabolites of tamoxifen, the effective reaction temperature and time were shown to be at 50 ℃ for 30 min. The 4-hydroxytamoxifen, which is known to major metabolite of tamoxifen, was not detected in human urine, whileas the hydroxymethoxytamoxifen was detected. We thought that this result was from the single dose of tamoxifen.

Comparison of the Volatile Components in Two Chinese Wines, Moutai and Wuliangye

Joo-Shin Kim,Shuk Fan Kam,Hau Yin Chung 한국응용생명화학회 2009 Journal of Applied Biological Chemistry (J. Appl. Vol.52 No.3

Volatile and odorous components in two Chinese wines, Moutai and Wuliangye, were partially investigated by direct solvent extraction. Sample extracts were analyzed by gas chromatography/mass spectrometry and gas chromatography-olfactometry. Fifty-six and thirty-eight compounds were found in Moutai and Wuliangye, respectively, including esters (19, 20), alcohols (8, 7), acids (6, 3), furans (5, 2), acetals (5, 2), phenols (2, 2), ketones (7, 0) and miscellaneous compounds (4, 2). Based on olfactometry, ethyl acetate, furfural and 2-furanmethanol were perceived only in the Moutai whereas diethyl succinate was recognized only in the Wuliangye. However, 1,1- Diethyoxyehtane, ethyl hexanoate, ethyl benzoate and pentanoic acid were found in both wines. Volatile and odorous components in two Chinese wines, Moutai and Wuliangye, were partially investigated by direct solvent extraction. Sample extracts were analyzed by gas chromatography/mass spectrometry and gas chromatography-olfactometry. Fifty-six and thirty-eight compounds were found in Moutai and Wuliangye, respectively, including esters (19, 20), alcohols (8, 7), acids (6, 3), furans (5, 2), acetals (5, 2), phenols (2, 2), ketones (7, 0) and miscellaneous compounds (4, 2). Based on olfactometry, ethyl acetate, furfural and 2-furanmethanol were perceived only in the Moutai whereas diethyl succinate was recognized only in the Wuliangye. However, 1,1- Diethyoxyehtane, ethyl hexanoate, ethyl benzoate and pentanoic acid were found in both wines.

Exploring the Metabolomic Responses of Bacillus licheniformis to Temperature Stress by Gas Chromatography/Mass Spectrometry

( Zixing Dong ),( Xiaoling Chen ),( Ke Cai ),( Zhixin Chen ),( Hongbin Wang ),( Peng Jin ),( Xiaoguang Liu ),( Kugenthiren Permaul ),( Suren Singh ),( Zhengxiang Wang ) 한국미생물생명공학회(구 한국산업미생물학회) 2018 Journal of microbiology and biotechnology Vol.28 No.3

Owing to its high protein secretion capacity, simple nutritional requirements, and GRAS (generally regarded as safe) status, Bacillus licheniformis is widely used as a host for the industrial production of enzymes, antibiotics, and peptides. However, as compared with its close relative Bacillus subtilis, little is known about the physiology and stress responses of B. licheniformis. To explore its temperature-stress metabolome, B. licheniformis strains ATCC 14580 and B186, with respective optimal growth temperatures of 42℃ and 50℃, were cultured at 42℃, 50℃, and 60℃ and their corresponding metabolic profiles were determined by gas chromatography/mass spectrometry and multivariate statistical analyses. It was found that with increased growth temperatures, the two B. licheniformis strains displayed elevated cellular levels of proline, glutamate, lysine, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, and octadecanoic acid, and decreased levels of glutamine and octadecenoic acid. Regulation of amino acid and fatty acid metabolism is likely to be associated with the evolution of protective biochemical mechanisms of B. licheniformis. Our results will help to optimize the industrial use of B. licheniformis and other important Bacillus species.

국화 ‘백마’(Chrysanthemum morifolium) 줄기로부터glycosyl glyceride 의 분리 및 동정

오현지,김형근,박하승,백윤수,권오근,신학기,백남인 한국응용생명화학회 2018 Journal of Applied Biological Chemistry (J. Appl. Vol.61 No.2

The stem of Chrysanthemum morifolium, ‘Baekma’, were repeatedly extracted with 80% aqueous MeOH and the concentrates was partitioned into ethyl acetate (EtOAc), n-butyl alcohol and H2O fraction. The repeated silica gel and octadecyl silica gel column chromatographies for the EtOAc fractions led to isolation of two glycosyl glycerides. The chemical structures of the compounds were determined as (2S)-1-O-β-D-galactopyranosyl- 2,3-dilinoleoylglycerol (1) and (2S)-1-O-β-D-galactopyranosyl- 2,3-dipalmitoylglycerol (2) based on spectroscopic data anlyses including nuclear magnetic resonance, mass sperctrometry, and infrared spectrometry and gas chromatography mass spectrometry. 국화(C. morifolium)품종인 ‘백마’ 줄기를 80% MeOH 수용액으로 3회 반복 추출한 뒤, 감압농축한 추출물을 EtOAc, n-butyl alcohol과 H2O층으로 계통분획을 실시하였다. EtOAc분획에 대하여 SiO2 및 ODS column chromatography를 반복실시하여 2 종의 지방산 화합물을 분리 및 정제하였다. Nuclear magnetic resonance, infrared spectrometry, FAB-MS, GC-MS data를 해석하여, 화합물 1과 2를 각각 (2S)-1-O-β-D-galactopyranosyl- 2,3-dilinoleoylglycerol과 (2S)-1-O-β-D-galactopyranosyl-2,3- dipalmitoylglycerol로 구조동정 하였다.

Identification and quantification of seven volatile n-nitrosamines in cosmetics using gas chromatography/chemical ionization-mass spectrometry coupled with head space-solid phase microextraction

Choi, N.R.,Kim, Y.P.,Ji, W.H.,Hwang, G.S.,Ahn, Y.G. Pergamon Press ; Elsevier Science Ltd 2016 Talanta Vol.148 No.-

<P>An analytical method was developed for the identification and quantification of seven volatile n-nitrosamines (n-nitrosodimethylamine [NDMA], n-nitrosoethylmethylamine [NMEA], n-nitrosodiethylamine [NDEA], n-nitrosodipropylamine [NDPA], n-nitrosodibutylamine [NDBA], n-nitrosopiperidine [NPIP], and n-nitrosopyrrolidine [NPYRD]) in water insoluble cream type cosmetics. It was found that the head space-solid phase microextraction (HS-SPME) was suitable for extraction, clean up, and pre-concentration of n-nitrosamines in the cream type samples so its optimal conditions were investigated. Identification and quantification of n-nitrosamines using single quadrupole gas chromatography/mass spectrometry (GC/MS) in chemical ionization (CI) mode were carried out with accurate mass measurements. Their accurate masses of protonated molecular ions were obtained within 10 mDa of the theoretical masses when sufficiently high signal was acquired from the unique calibration method using mass and isotope accuracy. For the method validation of quantification, spiking experiments were carried out to determine the linearity, recovery, and method detection limit (MDL) using three deuterated internal standards. The average recovery was 79% within 20% relative standard deviation (RSD) at the concentration of 50 ng/g. MDLs ranged from 0.46 ng/g to 36.54 ng/g, which was satisfactory for the directive limit of 50 ng/g proposed by the European Commission (EC). As a result, it was concluded that the method could be provided for the accurate mass screening, confirmation, and quantification of n-nitrosamines when applied to cosmetic inspection. (C) 2015 Elsevier B.V. All rights reserved.</P>