• Title/Summary/Keyword: gas chromatography-mass spectrometry

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Simultaneous Determination of Preservatives in Food by GC/MS (Gas Chromatography/Mass Spectrometry를 이용한 식품보존료의 동시분석방법 연구)

  • 김승기;노동석
    • Journal of Food Hygiene and Safety
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    • v.14 no.2
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    • pp.140-145
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    • 1999
  • Analytical method for preservatives in food was developed using gas chromatography/mass spectrometry (GC/MS). Propionic acid, sorbic acid, benzoic acid, ethyl salicylate, ethyl p-hydroxy benzoate, iso-propyl p-hydroxy benzoate, n-propyl p-hydroxy benzoate, iso-butyl p-hydroxy benzoate, n-butyl p-hydroxy benzoate, p-hydroxy benzoic acid and dehydro acetic acid were extracted from cooling beverage with diethyl ether. The polar hydroxyl and carboxyl groups of food preservatives were derivatized with N-methyl-N-tert-butyldimethylisilyl-trifluoroscetamide (MTBSTFA) to form the corresponding tert-bytyldimethyl-silylated derivatives, and submitted to GC/MS analysis. The mass spectra of the derivatives were investigated for the selection of monitoring ions for multi-residue analysis of 11 preservatives by GC/MS. The macro program was also developed for the qualitative analysis of these preservatives in food.

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Urinary Metabolism and Excretion of Carbinoxamine after Oral Administration to Man

  • Jung, Byung-Hwa;Chung, Bong-Chul;Park, Jong-Sei
    • Biomolecules & Therapeutics
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    • v.4 no.3
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    • pp.251-256
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    • 1996
  • The metabolism of carbinoxamine, 2-[(4-chlorophenyl)-2-pyridinyl-methoxy]-N, N-dimethylethaneamine, was studied in adult male volunteers after an oral dose of 15 mg. Solvent extracts of urine obtained with or without enzyme hydrolysis were analyzed by gas chromatography-mass spectrometry after derivatization with MSTFA/TMSCl (N-methyl-N-trimethylsilyltrifluoroacetamide/trimethyl chlorosilane). The structures of metabolites were determined based on the electron impact (EI) and chemical ionization (CI) mass spectra. Nonconjugated metabolites identified in the urine were carbinoxamine, nor-carbinoxamine, and bits-nor-carbinoxamine. Parent drug, nor-carbinoxamine, and bits-nor-carbinoxamine were also detected as conjugated forms. These metabolites observed in human urine were different from those previously reported in the rat. Urinary excretions of carbinoxamine were reached to maxima in 4 hours after drug administration with 4.9%-8.1% and 2.5-4.2% of the dose excreted during 24 h as carbinoxamine and its glucuronide, respectively.

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Determination of panthenol, cholecalciferol and tocopherol in cosmetic products by gas chromatography-mass spectrometry in SIM mode

  • Hye-Jin Jeong;Myo
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.22 no.2
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    • pp.153-160
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    • 1996
  • A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

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Simultaneous Determination of 4-Nitrotoluene and Benzophenone in Ground Water and Soil by Gas Chromatography-Mass Spectroscopy

  • Kwon, Oh-Seung;Kim, Eun-Young;Ryu, Jae-Chun
    • Analytical Science and Technology
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    • v.16 no.1
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    • pp.59-69
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    • 2003
  • Benzophenone (BZP) and 4-nitrotoluene (4-NT) listed as endocrine disrupting chemicals are suspected to contaminate ground water sites and soil. Analytical method for simultaneous determination of the two chemicals in soil and ground water was developed by gas chromatography-mass spectrometry. Water (100 ml) was extracted with hexane, and soil (10 g) was extracted with methanol and hexane. Recovery in water was >72% for BZP and 90-118% for 4-NT. Recovery for 4-NT and BZP in soil was 51-59% with coefficient variation of less than 19.5%. Calibration curves showed a good linearity with $r^2=0.997$. In water and soil collected at nation-wide sites, BZP was found at 5 sites among 43 water sites at the concentration of $14.87{\pm}3.83ng/100 ml$. No 4-NT was found. It is suggested that this method is appropriate to the simultaneous quantitation of 4-NT and BZP in ground water and soil samples.

Simultaneous detection of five biocides in household products by gas chromatography-mass spectrometry

  • Choi, Kyeong-Yun;Lim, Hyun-Hee;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.197-204
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    • 2022
  • A gas chromatography-mass spectrometric method was developed for determining 5-chloro-2-methyl-4-isothiazolin-3-one (CMIT), 2-methyl-4-isothiazolin-3-one (MIT), 1,2-benzisothiazolin-3-one (BIT), 3-iodo-2-propynyl butyl carbamic acid (IPBC) and benzoic acid (BA) in household products. A 0.5 g sample was placed in a test tube and dissolved with 5 mL water, 5 mL methylene chloride and 1.0 mL methanol. The solution was extracted by ultra-sonication followed by mechanical shaking using the salting out effect. Under the established condition, the lowest quantification limits of all analytes were in the range of 0.04-10 mg/kg and their relative standard deviations were less than 8.0 %. The method was used to analyze 10 household products. As a result of analyzing 10 household products, MIT was detected in the range of 1.2-3.5 mg/kg in 3 of 10 samples, CMIT was detected in the range of 2.6-8.2 mg/kg in 3 of 10 samples, and BA was detected in the range of 5.0-15 mg/kg in 4 of 10 samples. Meanwhile, BIT and IPBC were not detected in any of the products. It has been shown that this method can be used for the simultaneous determination of biocides with various physical and chemical properties in household products.

Identification of Homoserine Lactone Derivatives Using the Methionine Functionalized Solid Phase Synthesis by Gas Chromatography/Mass Spectrometry

  • Moon, Hong-Sik
    • Archives of Pharmacal Research
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    • v.27 no.1
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    • pp.25-30
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    • 2004
  • Combinatorial homoserine lactone mixtures and individual products were obtained from the methionine-functionalized resin in solid-phase synthesis. The four-step process consisting of a coupling step of an N-Fmoc-L-methionine, deprotection of N-Fmoc group, N-coupling with a carboxylic acid, and cleavage reaction through a polymer supported strategy is described. Gas chromatography-mass selective detector (GC-MSD) techniques provide the most powerful methods for identifying both the combinatorial mixtures and individual products.

MEASUREMENT OF PESTICIDES RESIDUES USING SPECTROSCOPY ON AGRICULTURAL PRODUCTS

  • Kim, Y. W.;S. H. Noh
    • Proceedings of the Korean Society for Agricultural Machinery Conference
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    • 2000.11c
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    • pp.525-532
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    • 2000
  • A new spectroscopic method for pesticide residues detection on agricultural products was developed. The general determination methods are high performance liquid chromatography (HPLC), gas chromatography (GC) or GC-mass spectrometry. They have provided relatively good detection limit and accuracy with complicated and time-consuming (5hrs above) procedures. In addition freshness is very important for evaluating qualities of agricultural products. This requires a simple and fast method for detection of pesticides. Reflectance, transmittance and fluorescence spectrometry of pesticides were tested using UV range because most of pesticides contain conjugation band in the molecular structures. Fluorescence spectrometry showed better sensitive to detect pesticide residues than did reflectance and transmittance spectrometry. Intensity and shape of fluorescence spectra showed different patterns with different structures of pesticides. Detection limit for fluorescence spectrometry was 0.1 ppm to 10 ppm depending on the structures of pesticides. Application of fluorescence spectrometry appears to be an easy method for detection of pesticide residues on agricultural products.

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Headspace gas chromatographic analysis as an objective method for measuring rancidity in soybean oil (Headspace 가스크로마토그라피를 이용한 대두유 산화진행도의 객관적 평가방법)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.154-161
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    • 1991
  • An objective method for measuring rancidity in soybean oil was developed based on the volatile contents obtained by headspace gas chromatographic analysis. Apparatus for headspace volatile cold trapping-thermal desorption was described, designed to collect and analyze volatiles of soybean oil. Samples of commercially processed soybean oil were stored under controlled condition and then evaluated for flavor by a eight member trained panel and for volatile contents by headspace gas chromatographic analysis. Twenty-three GC peaks were identified on the basis of relative retention time of reference compounds and gas chromatography-mass spectrometry. The volatile compounds identified were autoxidation products of principal unsaturated fatty acids of soybean oil. The simple linear regressions of flavor score with the pentanal or hexanal contents in aged soybean oil gave correlation coefficient of 0.990 and 0.994. respectively. Pentanal and hexanal contents could be used as a potentially useful index for predicting flavor scores of soybean oil.

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Identification of Volatile Flavor Components of Chinese chive and Baek-Seok Chie (중국 부추와 백석 부추의 휘발성 풍미 성분의 동정)

  • 이혜정;박희옥
    • The Korean Journal of Food And Nutrition
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    • v.10 no.4
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    • pp.539-543
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    • 1997
  • This study was carried out to investigate the Chinese and Baek-Seok chive. We collect the volatile components of Chinese and Baek-Seok chive by dynamic head space method. Chinese chive was analyzed by Gas chromatography-Mass Spectrometry(GC-MS). 28 components including 20 sulfides, 5 alcohols, 1 benzene and 2 aldehydes compounds were identified in samples, Also Baek-Seok chive was analyzed by GC-MS. 32 components including 19 sulfides, 10 alcohols, 2 benzonoides and 1 aldehyde compounds were confirmed.

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