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

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Analytical Method Development and Monitoring of Residual Solvents in Dietary Supplements (건강기능식품 중 잔류용매 분석법 개발 및 모니터링)

  • Lee, Hwa-Mi;Shin, Ji-Eun;Jang, Young-Mi;Kim, Hee-Yun;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.42 no.4
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    • pp.390-397
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    • 2010
  • Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.

Identification of Irradiation-induced Volatile Flavor Compounds in Beef (방사선 조사 쇠고기에서의 휘발성 조사물질의 구명)

  • Cha, Yong-Jun;Kim, Hun;Park, Sung-Young;Kim, So-Jung;You, Young-Jae
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.29 no.6
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    • pp.1042-1049
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    • 2000
  • Irradiation-induced volatile flavor compounds in irradiated (1, 3, 5, 10 kGy) beef were analyzed by liquid liquid continuous extraction (LLCE) and gas chromatography/mass spectrometry (GC/MS) methods. One hundred fifty volatile compounds were detected in irradiated beef. These compounds were composed mainly of 71 hydrocarbons, 35 aromatic compounds, 15 aldehydes, 7 ketones, 4 acids, 6 esters and 12 miscellaneous compounds. Among these, only 6 volatile compounds including (E) -2-hexenal, nonene, 2-nonenal, cyclodecene, dodecene and cyclododecene were detected as irradiation-induced volatile flavor compounds, comparing with unirradiated beef meat. However, 4 volatile compounds, such as cyclodecene (r=0.88), (E)-2-hexenal (r=0.85), nonene (r=0.74) and 2-nonenal (r=0.70), having a positive correlation coefficient with the increment of irradiation dose, were considered as marker compounds for detecting irradiation dosages in irradiated beef.

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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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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.

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.

The analysis of ethylene glycol and metabolites in biological specimens (생체시료에서 에틸렌 글리콜과 그 대사체 분석에 관한 연구)

  • Park, Seh-Youn;Kim, Yu-Na;Kim, Nam-Yee
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.69-77
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    • 2011
  • Ethylene glycol (EG) is produced commercially in large amounts and is widely used as antifreeze or deicing solution for cars, boats, and aircraft. EG poisoning occurs in suicide attempts and infrequently, either intentionally through misuse or accidental as EG has a sweet taste. EG has in itself a low toxicity, but is in vivo broken down to higher toxic organic acids which are responsible for extensive cellular damage in various tissues caused principally by the metabolites glycolic acid and oxalic acid. The most conclusive analytical method of diagnosing EG poisoning is determination of EG concentration. However, victims are sometimes admitted at a late stage to hospitals or died during emergency treatment like a gastric lavage or found rotten dead, when blood EG concentrations are low or not detected. Therefore, in this study, the identification of EG was not only performed by gas chromatograpyc-mass spectrometry (GC-MS) following derivatization but also further toxicological analyses of metabolites, glycolic acid (GA) and oxalic acid (OA), were performed by ion chromatography in various biological specimens. A ranges of blood concentrations (3 cases) was $10\sim2,400\;{\mu}g/mL$ for EG, $224\sim1,164\;{\mu}g/mL$ for GA and ND $\sim40\;{\mu}g/mL$ for OA, respectively, In other biological specimens (liver, kidney, bile and pleural fluid), a range of concentrations (3 cases) was ND $\sim55,000\;{\mu}g/mL$ for EG, ND $\sim1,124\;{\mu}g/mL$ for GA and ND $\sim60\;{\mu}g/mL$ for OA, respectively. Liver and kidney tissues were recommended specimens including blood because OA, a final metabolite of EG, was identified large amounts in these despite no detectable EG caused by some therapy.

Volatile Flavor Properties of Hallabong Grown in Open Field and Green House by GC/GC-MS and Sensory Evaluation (노지 및 시설에서 재배된 한라봉의 기기분석 및 관능평가에 의한 향기특성)

  • Song, Hee-Sun;Park, Yeon-Hee;Moon, Doo-Gyung
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.34 no.8
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    • pp.1239-1245
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    • 2005
  • Hallabong peel oils grown in open field and green house were extracted by hand-pressing flavedo and collected on ice. Volatile flavor components of Hallabong peel oils were identified and compared by using gas chromatography and mass- spectrometry. Forty-four flavor components were identified in open field oil and 45 flavor components in green house oil. (E) -Limonene-1,2-epoxide and neral were identified only in Hallabong oil grown in open field, on the other hand, $\beta$-cubebene, $\beta$-elemene and decyl acetate were detected only in green house oil. Limonene was the most abundant component in both oils as more than 86$\%$ of peak weight, followed by sabinene (1.8$\~$ 3.6$\%$) and myrcene (2.4$\~ $2.6$\%$). The difference of the volatile profile between open field and green house oils were significantly characterized by identification and quantity of alcohol group. The total alcohols in open field and green house oils accounted for 1.8$\%$ and 0.8$\%$, respectively. Among alcohols, the level of linalool was relatively high in open field oil (1.2$\%$), however, it accounted for 0.5$\%$ in green house oil. Flavor properties of fresh Hallabong peel and flesh were also examined by sensory evaluation. Flavor properties of fresh Hallabong grown in open field were relatively stronger on both peel and flesh by sensory analysis. Sweetness was strong in Hallabong flesh from open field, and sourness in that from green house. The sensory evaluation of the preference in consideration of taste and aroma was significantly high in Hallabong grown in open field (p<0.01). From the present study, the stronger flayer properties and the preference of Hallabong from open field by sensory evaluation seem to be associated with the high level of linalool in its peel oil, and the composition of monoterpene hydrocarbons such as sabinene and (E) -$\beta$ -ocimene.