• Title/Summary/Keyword: Gas Chromatography/mass spectrometry

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Studies on Photosensitized Oxidation in the Lipids of Irish moss, Laver and Oyster (진두발, 김 및 굴의 지질에 있어서 광증감 산화에 관한 연구)

  • KIM Kui-Shik;KOIZUMI Chiaki;BAE Tae-Jin
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.30 no.3
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    • pp.355-360
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    • 1997
  • In order to investigate the influence of photosensitized oxidation in the sun-dried irish moss (Chondrus Ocellatus), laver (Porphyra Yezoensis) and ultra violet irradiated oyster (Crassostrea gigas) the oxidation of lipid and isomers of hydroperoxides were analyzed by gas chromatography-mass spectrometry. The lipid contents of oyster, irish moss and layer were $2.7\%,\;0.1\%,\;0.1\%$ of respectively. Peroxide value, 56,7 meq/kg in the raw oyster was increased of 100.9 meq/kg by the U.V, irradiation for 4 hours. Also the peroxide values of the irish moss and laver were increased by the sun-drying. In the identification of hydroperoxides isomers by trimethylsily (TMS) derivative of photo-oxidized lipid from oyster, irish moss and laver, the proportions of positional isomer, 9-OOH and 13-OOH were dominant than those 10-OOH and 12-OOH.

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Changes in Organic acids, Free Sugars, and Volatile Flavor Compounds in Fig (Ficus carica L.) by Maturation Stage (무화과의 성숙도에 따른 유기산, 유리당 및 향기 성분의 변화에 관한 연구)

  • Shin, Tai-Sun;Park, Jin-A;Jung, Bok-Mi
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.7
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    • pp.1016-1027
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    • 2015
  • This study collected 120 figs, classified them into six degrees of maturity according to hardness values, and analyzed contents of organic acids and free sugars. Volatile compounds in figs were investigated using the solid-phase microextraction method of gas chromatography/mass spectrometry. For measurement of texture, elasticity increased up to stage 4 and decreased again. Cohesiveness and brittleness increased with maturation. Organic acids in figs were mainly composed of citric acid, malic acid, and tartaric acid in the final stage. Fructose and glucose were the major sugar components of figs. Fructose content decreased from stage 1 to stage 4 and then increased significantly. One hundred and nineteen volatile compounds were identified in figs, and classes were 14 acids, 15 alcohols, 23 aldehydes, 10 esters, 33 hydrocarbons, 11 ketones, four aromatics, six miscellaneous, and five terpenes. The dominant volatile components in figs were hexadecanoic acid, hexane, dodecanal, DL-limonene, 2-hexanal, nonanal, and 6-methyl-5-hepten-2-one.

Comparison of Volatile Compounds Identified in Different Parts of Peucedanum japonicum Thunberg by Harvest Time (방풍나물의 수확시기에 따른 부위별 향기성분 비교 분석)

  • Jung, Bok-Mi;Shin, Tai-Sun;Heo, Young-Ran
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.12
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    • pp.1871-1880
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    • 2014
  • Headspace volatile compounds of leaf, stem, and root of Peucedanum japonicum Thunberg (PJT) harvested in March and July were isolated, separated, and identified by using a combined system of solid phase microextraction and gas chromatography/mass spectrometry. Identified numbers of volatile compounds were 72, 75, and 63 in March PJT as well as 78, 73, and 69 in July, respectively. Total compounds identified from PJT consisted of alcohols (1~7), aldehydes (7~15), esters (1~4), hydrocarbons (5~9), ketones (1~2), monoterpenes (13~16), monoterpene alcohols (1~5), monoterpene aldehydes (2~4), monoterpene esters (1~4), monoterpene ketones (1~2), sesquiterpenes (16~24), and miscellaneous compounds (2~3). Major volatile compounds of PJT were monoterpenes at all harvest times and in all parts of PJT. The amounts of ${\beta}$-pinene in leaf and stem harvested in March were highest in monoterpenes, followed by ${\alpha}$-pinene and ${\beta}$-myrcene. However, amounts of volatile compounds of monoterpenes in leaf and stem from July PJT were in the decreasing order of ${\beta}$-pinene, ${\beta}$-phellandrene, and ${\beta}$-myrcene. Of the 39 sesquiterpenes identified in PJT, (E)-caryophyllene in March leaf was the most abundant volatile compound, followed by acoradiene in March leaf, ${\beta}$-elemene, and ${\alpha}$-copaene in July stem.

Identification of the Volatile Components in Korean Ordinary Kochujang (한국재래식(韓國在來式) 고추장의 향기성분동정(香氣成分同定))

  • Ahn, Cheol-Woo;Kim, Jong-Kyu;Sung, Nack-Kie
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.16 no.3
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    • pp.27-34
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    • 1987
  • The present paper was attempted to obtain the basic date concerning a reasonable preparing method and optimum fermentation conditions of Kochujang (Red pepper paste). To establish the standard quality of Kochujang, the chemical compositions and the volatile components of Kochujang was discussed. The native Kochujang collected from 80 households contained 40.51% of moisture, 6.00% of salts, 3.25 % of crude fat, 10.30 % of crude ash, pH 4.79, 9.28ml of tillable acidity. 19.60% of reducing sugar, 179.51 mg/100g of amino nitrogen and 4.43% of total nitrogen. The volatiles of Kochujang were extracted by a steam-distillation under the reduced pressure and determined by gas chromatography-mass spectrometry (GC-MS). Total volatile components identified in the native Kochujang were 46 components, i. e., 30 components in neutral fraction, 8 components in phenolic fraction and 8 components in acidic fraction, respectively. But no components were detected basic fraction.

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Identification of Irradiation -induced Volatile Marker Compounds in Irradiated Red Pepper Powder (방사선조사 고추가루로부터 휘발성 표지물질의 구명)

  • Kim, Hun;Ahn, Jun-Suck;Sin, Yeong-Min;Lee, Yong-Ja;Lee, Kyung-Hae;Byun, Myung-Woo;Cha, Yong-Jun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.2
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    • pp.236-242
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    • 2005
  • To develop a new detection method using irradiation-induced volatile marker compounds of red pepper powder (RP), the volatile compounds of irradiated RP (0, 1, 3, 5, and 10 kGy) were analyzed by purge and trap (P&T)/solid phase microextraction (SPME)/gas chromatography/mass spectrometry (GC/MS) methods. A total of 51 and 31 compounds were detected in IRP by SPME and P&T methods, respectively. Among these, 25 compounds, which were composed of 4 hydrocarbons, 7 aldehydes, 1 ketone, 3 alcohols, 4 aromatic compounds, 2 esters and 4 miscellaneous compounds, showed irradiation dependent manner with significant positive correlation (p<0.01 or p<0.05) between irradiation dose and relative concentration. However, all compounds except 1,3-bis(1,1-dimethylethyl)benzene were not suitable as marker compounds because of their low determination coefficients ($R^2$<0.80) between irradiation dose and their concentrations, and detectablilty in nonirradiated sample. Therefore, only one compound, 1,3-bis(1,1-dimethylethyl)benzene, was tentatively identified as a volatile marker compound to detect irradiated RP.

Essential Oil Isolated from Iranian Yarrow as a Bio-rational Agent to the Management of Saw-toothed Grain Beetle, Oryzaephilus surinamensis (L.) (머리대장가는납작벌레의 합리적 방제 물질로 이란 서양가새풀 정유의 살충효과 평가)

  • Ebadollahi, Asgar
    • Korean journal of applied entomology
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    • v.56 no.4
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    • pp.395-402
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    • 2017
  • Overuse of synthetic pesticides caused negative side-effects such as environmental contamination, development of insect pests' resistance, and effects on non-target organisms. Plant origin substances without/or with low mammalian toxicity have been considered as promising alternatives to the synthetic pesticides. Fumigant toxicity of the essential oil of Iranian Yarrow, Achillea millefolium L., was investigated against a cosmopolitan stored-product insect pest: saw-toothed grain beetle (Oryzaephilus surinamensis L.). Chemical profile of this essential oil was studied by Gas Chromatography-Mass Spectrometry. Tested concentrations were significantly effective to the mortality of insect pest. A positive correlation between essential oil concentrations and pest mortality were realized. LC50 value (lethal concentration needed to 50% mortality) was achieved as $17.977(16.195{\pm}20.433){\mu}l/l$ air. The main components were 1,8-Cineole (13.17%), nerolidol (12.87%), ${\alpha}$-cubebene (12.35%), artemisia ketone (6.69%), ${\alpha}$-terpineol (5.27%), alloaromadendrene oxide (4.71%) and borneol (3.99%). Terpenic compounds including monoterpene hydrocarbons (8.19%), monoterpenoids (44.23%), sesquiterpene hydrocarbons (21.69%) and sesquiterpenoids (22.24%) were 96.35% of the total identified compounds. Results indicated that the terpene-rich A. millefolium essential oil may be considered as a safe bio-agent in the O. surinamensis management.

Analysis of Methamphetamine and Amphetamine in Oral Fluid of Eleven Drug Abusers (마약남용자 11명의 타액 중 메스암페타민의 분석)

  • Kim, Eun-Mi;Lee, Ju-Seon;Choi, Hye-Young;Choi, Hwa-Kyung;Chung, Hee-Sun
    • YAKHAK HOEJI
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    • v.52 no.6
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    • pp.419-425
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    • 2008
  • A qualitative and quantitative analytical method was developed for detection of methamphetamine (MA) and its main metabolite amphetamine (AM) in oral fluid. Oral fluids of eleven drug abusers were provided by Police, specimens were collected by stimulation with a cotton swab treated with 20 mg of citric acid ($Salivette^{(R)}$; Sarstedt, USA). As the preliminary test, oral fluid samples were screened for amphetamines by Fluorescence Polarization Immunoassay (TDxFLx, Abbott Co.). Extraction for MA was performed using solid-phase extraction (SPE) by $RapidTrace^{TM}$ (Zymark, USA) with mixed mode cation exchange cartridge, CLEAN $SCREEN^{(R)}$ (130 mg/3 ml, UCT) after dilution with phosphate buffer. Samples were evaporated and derivatized by pentafluoropropionic acid anhydride (PFPA). Quantitation of MA and AM was performed by gas chromatography-mass spectrometry (GC-MS) using selective ion monitoring (SIM), the quantitation ions were m/z 204 (MA), 208 (MA-$D_5$), 190 (AM) and 194 (AM-$D_5$). The selectivity, linearity of calibration, limit of detection (LOD) and quantification (LOQ) within- and between day precision, accuracy and recoveries were examined as parts of the method validation. All oral fluid samples gave positive results to immunoassay for MA (cut-off level, 50 ng/ml as d-amphetamine). Concentrations of MA and AM by GC-MS in eleven samples were ranged 104.2${\sim}$4603.3 ng/ml and 32.4${\sim}$268.6 ng/ml, respectively. Extracted calibration curves of MA and AM were linear over the two concentration range of 1${\sim}$100 and 50${\sim}$1000 ng/ml with correlation coefficient of above 0.999. LOQ of MA and AM was 1 and 3 ng/ml, respectively. The intraand inter-day run precisions (CV) for MA and AM were less than 10%, and the accuracies (bias) for MA and AM were also less than 10% at the two different concentrations 5 and 100 ng/ml at low calibration range, 50 and 1000 ng/ml at high calibration range. The absolute recoveries of MA and AM at low and high calibration ranges were more than 82% and 75%, respectively. In this study the qualitative and quantitative analytical method of MA in oral fluid was established. Oral fluid testing may detect drug use in past hours because of its shorter detection window than urine, and be useful in post-accident situations. So oral fluids will be most useful for testing drug abuse in the driving under the influence of drug (DUID) as the alternative specimens of urine.

Comparative analysis of the transcriptomes and primary metabolite profiles of adventitious roots of five Panax ginseng cultivars

  • Lee, Yun Sun;Park, Hyun-Seung;Lee, Dong-Kyu;Jayakodi, Murukarthick;Kim, Nam-Hoon;Lee, Sang-Choon;Kundu, Atreyee;Lee, Dong-Yup;Kim, Young Chang;In, Jun Gyo;Kwon, Sung Won;Yang, Tae-Jin
    • Journal of Ginseng Research
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    • v.41 no.1
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    • pp.60-68
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    • 2017
  • Background: Various Panax ginseng cultivars exhibit a range of diversity for morphological and physiological traits. However, there are few studies on diversity of metabolic profiles and genetic background to understand the complex metabolic pathway in ginseng. Methods: To understand the complex metabolic pathway and related genes in ginseng, we tried to conduct integrated analysis of primary metabolite profiles and related gene expression using five ginseng cultivars showing different morphology. We investigated primary metabolite profiles via gas chromatography-mass spectrometry (GC-MS) and analyzed transcriptomes by Illumina sequencing using adventitious roots grown under the same conditions to elucidate the differences in metabolism underlying such genetic diversity. Results: GC-MS analysis revealed that primary metabolite profiling allowed us to classify the five cultivars into three independent groups and the grouping was also explained by eight major primary metabolites as biomarkers. We selected three cultivars (Chunpoong, Cheongsun, and Sunhyang) to represent each group and analyzed their transcriptomes. We inspected 100 unigenes involved in seven primary metabolite biosynthesis pathways and found that 21 unigenes encoding 15 enzymes were differentially expressed among the three cultivars. Integrated analysis of transcriptomes and metabolomes revealed that the ginseng cultivars differ in primary metabolites as well as in the putative genes involved in the complex process of primary metabolic pathways. Conclusion: Our data derived from this integrated analysis provide insights into the underlying complexity of genes and metabolites that co-regulate flux through these pathways in ginseng.

Identification of volatile flavor compounds in Jeju citrus fruits (제주감귤류의 휘발성 향기성분의 확인)

  • Hong, Young Shin;Kim, Kyong Su
    • Food Science and Preservation
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    • v.23 no.7
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    • pp.977-988
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    • 2016
  • The volatile flavor compounds in five Jeju citrus fruit varieties (Cheonhyehyang, Hallabong, Jinjihyang, Hwanggeum hyang and Redhyang) were extracted by simultaneous distillation-extraction (SDE) using solvent mixture of n-pentane and diethyl ether (1:1, v/v) and analyzed by using gas chromatography-mass spectrometry (GC-MS). The number of aroma compounds were identified with : 104 (4,939.77 mg/kg) in Cheonhyehyang, 98 (3,286.38 mg/kg) in Hallabong, 105 (3,317.56 mg/kg) in Jinjihyang, 102 (4,293.39 mg/kg) in Hwanggeumhyang, and 108 (4,049.94 mg/kg) in Redhyang. The detected main volatile compounds were; limonene, sabinene, ${\beta}$-myrcene, ${\alpha}$-pinene, ${\beta}$-pinene, linalool, 4-terpineol, ${\alpha}$-terpineol, (E)-${\beta}$-ocimene and ${\gamma}$-terpinene. Among the identified volatiles compounds, ethyl-benzene, nonanol, 1-p-menthen-9-al, (E)-isocarveol, methyl salicylate, ${\alpha}$-terpinen-7-al, perilla alcohol, and ethyl-dodecanoate were detected in Cheonhyehyang. only Furthermore, ${\beta}$-chamigrene and ${\alpha}$-selinene were in Hallabong only; 3-hydroxybutanal, (E)-2-nonenal, isoborneol, octyl acetate, (E)-2-undecenal, ${\beta}$-ylangene and guaia-6,9-diene in Jinjihyang. ${\rho}$-Cymenene, ${\beta}$-thujone, selina-4,11-diene and (E,E)-2,6-farnesol in Hwanggeumhyang only; and ${\rho}$-cymen-8-ol, bornyl acetate, carvacrol, bicycloelemene, ${\alpha}$-cubebene and 7-epi-${\alpha}$-selinene in Redhyang only. This study confirmed the differences in composition and content of volatile aroma components in five varieties of Jeju citrus fruits.

Method Development and Validation of Strychnine in Blood by Gas Chromatography/Mass Spectrometry Using Solid Phase Extraction and its Application in Real Specimens (SPE 및 GC/MS에 의한 혈액중 스트리크닌의 분석법 개발 및 검출사례)

  • Rhee, Jongsook;Yum, Hyesun;Moon, Sungmin;Lee, Sangki
    • YAKHAK HOEJI
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    • v.57 no.2
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    • pp.87-94
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    • 2013
  • An analytical methodology based on solid-space extraction (SPE) with with Bond Elut Certify cartridge (Varian, 130 mg) has been developed for the qualification and quantitation of strychnine in blood. After the elution layer was evaporated, the residue was reconstituted with methanol for GC/MS. Internal standard was used 10 mg/l dextromethorphan. Strychnine is a potent central nervous stimulant and convulsant, and an alkaloid found in seeds of Strychnos nux-vomica. It was used therapeutically to improve circulation and muscle tone in oral or intramuscular doses of 0.05~8 mg. The fatal dose of strychnine for humans is 50~100 mg. A man was found dead lying curled up the corner of the large room in a roof house after the fire fighter opened a locked door inside to put out the fire. The postmortem blood and gastric contents were analyzed for toxicological testing. Strychnine and brucine were detected using GC/MS first in gastric contents extracts. The contents of strychnine was 0.083 mg/l in heart blood, 0.088 mg/l in peripheral blood and 4.0 mg/kg in gastric contents, respectively. Method validation was carried out in terms of linearity, accuracy, precision (intraday, interday) in blood. The assay is linear over 0.05~10 mg/l ($r^2$=0.999). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.02 mg/l (S/N=3) and 0.07 mg/l (S/N=10), respectively. Accuracy (bias%) of strychnine with 0.1, 1 and 10 mg/l was 12.0% (n=6), 9.3% (n=6) and 6.9% (n=6), respectively. Intraday precision (CV%) of strychnine with, 0.1, 1 and 10 mg/l were 6.4%, 10.4%, 1.2% (n=6), respectively. Interday precision (CV%) of strychnine with 0.1, 1 and 10 mg/l over three days were 24.0%, 18.5%, 13.8% (n=18), respectively. Relative recovery with 0.1, 1 and 10 mg/l (in blood) were 114.9%, 99.3% and 87.4% (n=6), respectively. The described method can be applied in forensic toxicology to determine strychnine in blood samples.