• Title/Summary/Keyword: GC-determination

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Determination of Miliacin from Proso Millet Oil by GC/MS (GC/MS를 이용한 기장 기름의 밀리아신 함량 분석)

  • Yeon Ju An;Byeong Won Lee;Ji Ho Chu;Seok Bo Song;Ji Young Kim;Young Kwang Ju;Sang Ik Han
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.67 no.4
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    • pp.335-341
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    • 2022
  • Proso millet (Pacnicum miliaceum L.) has a various of functional substances, so the demand is increasing as interest in human health benefits. In particular, miliacin, a triterpenoid in proso millet, is known to be effective in hair loss due to its promoting metabolism and proliferation of keratinocytes and showing protective effects from apoptosis. In this study, proso millet oil was extracted and analyzed by GC/MS using the extraction method of unsaponifiable substances after saponification reaction. The components of proso millet oil were confirmed through qualitative analysis by GC/MS. The miliacin content of 5 varieties of proso millet and 2 varieties of foxtail for comparison was analyzed. In the result, components of pentacyclic triterpenes such as β-amyrine and lupeol were detected in proso millet, and the content of miliacin was highest in Hallachal at 370.38±0.04 ㎍/100 mg oil. In addition, the content of miliacin was not detected in Samdachal and Samdamae, which are varieties of foxtail millet.

Validation and Determination of the Contents of Acetaldehyde and Formaldehyde in Foods

  • Jeong, Hye-Seung;Chung, Hyun;Song, Sang-Hoon;Kim, Cho-Il;Lee, Joon-Goo;Kim, Young-Suk
    • Toxicological Research
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    • v.31 no.3
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    • pp.273-278
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    • 2015
  • The aim of this study was to develop an efficient quantitative method for the determination of acetaldehyde (AA) and formaldehyde (FA) contents in solid and liquid food matrices. The determination of those compounds was validated and performed using gas chromatography-mass spectrometry combined by solid phase micro-extraction after derivatization with O-(2,3,4,5,6-pentafluoro-benzyl)-hydroxylamine hydrochloride. Validation was carried out in terms of limit of detection, limit of quantitation, linearity, precision, and recovery. Then their contents were analyzed in various food samples including 15 fruits, 22 milk products, 31 alcohol-free beverages, and 13 alcoholic beverages. The highest contents of AA and FA were determined in a white wine (40,607.02 ng/g) and an instant coffee (1,522.46 ng/g), respectively.

Simultaneous Determinaton of Octylphenol, Nonylphenol, Bis(2-ethylhexyl) phthalate in Biological Samples (생체시료 중 Octylphenol, Nonylphenol, Bis(2-ethylhexyl) phthalate의 동시정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.95-102
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    • 2001
  • A comprehensive analytical method of endocrine disruptors[i.e., nonylphenol(NP), octylphenol(OP), bis(2-ethylhexyl) phthalate(BEHP)] in meat or pork samples was developed. The method employed closed culture tube extraction with dichloromethane and solvent exchange to iso-hexane and SPE(2g) aminopropyl column, followed by determination on gas chromatography linked to mass spectrometry(GC/MS) operated in the single ion monitering(SIM) mode. For the multipoint recovery of nonylphenol, octylphenol and bis(2-ethlhexyl) phthalate OP, NP were showen good recoveries in $0.125-1.25{\mu}g/g$ range of concentration, and BEHP more good recoveries in $0.0125-12.5{\mu}g/g$ wide range of concentration. The present method was applied to beef or pork samples of mart and butcher in Cheonju city and near Cheonju. The range of concentrations was respectively, $0.06-0.24{\mu}g/g$ in nonylphenol(NP) and $0.36-2.35{\mu}g/g$ in bis(2-ethylhexyl) phthalate(BEHP), but octylphenol(OP) was not dected in any samples. This method provides a powerful analytical tool to investigate a wide range of endocrine disruptors in biological samples of limited quantity.

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Determination of Dimethyl Disulfide, Diallyl Disulfide, and Diallyl Trisulfide in Biopesticides Containing Allium Sativum Extract by Gas Chromatography

  • Lim, Sung-Jin;Lee, Ji-Hye;Kim, Jin-Hyo;Cho, Geun-Hyoung;Cho, Nam-Jun;Park, Byung-Jun
    • Korean Journal of Environmental Agriculture
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    • v.33 no.4
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    • pp.381-387
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    • 2014
  • BACKGROUND: Garlic (Allium sativum) extract has been allowed as commercial biopesticide material for pesticidal activity in the Environmentally-friendly Agriculture Promotion Act. Nine commercial biopesticides containing A. sativum extract have been marketed in Korea. However, the analytical method of the active substances in these materials has not been studied. METHODS AND RESULTS: Cartridge clean-up method for the determination of dimethyl disulfide(DMDS), diallyl disulfide(DADS), and diallyl trisulfide(DATS) in biopesticides containing A. sativum extract was developed and validated by gas chromatography(GC). The clean-up method was optimized using hydrophilic lipophilic balance (HLB) solid phase extraction(SPE) cartridges for the bioactive sulfides in biopesticides containing A. sativum extract, and the eluate was analyzed to quantify the DMDS, DADS, and DATS using the GC. The developed method was validated, and the LOQ and recovery rates of DMDS, DADS, and DATS were 0.226, 0.063, and $0.051mg\;L^{-1}$ and 80.6, 84.8, and 73.1%, respectively. From the nine commercial biopesticide samples, contents of DMDS, DADS, and DATS were analyzed using the developed method and results showed $2.3mg\;L^{-1}$, respectively. CONCLUSION: The developed method could be used in determining the quality of biopesticides for the manufacture of commercial biopesticides containing A. sativum extract.

Determination of 3-Monochloro-1, 2-propanediol in Acid Hydrolyzed Soysauce(Ganjang) by Gas-Chromatography with Electron Capture Detector (Gas Chromatography-Electron Capture Detector를 이용한 산분해간장중의 3-Monochloro-1, 2-propanediol 분석법에 관한 연구)

  • 최종동;문귀임;오현숙;김동술
    • Journal of Food Hygiene and Safety
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    • v.16 no.1
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    • pp.61-65
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    • 2001
  • To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

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Determination of hormonal active compounds in meat (육류 식품중 호르몬 성분의 분석)

  • Seo, Jungju
    • Analytical Science and Technology
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    • v.21 no.6
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    • pp.526-534
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    • 2008
  • To determine the trace level of synthetic and natural hormones in food, the improvement of official analytical method and new development of simultaneous determination of hormones were established. On the basis of developed analytical method, the background level of natural hormones and distribution of residual hormones were monitored in meat. Target hormones were six natural hormones such as estrogens ($17{\beta}$-estradiol, $17{\alpha}$-estradiol, estrone), androgens ($17{\beta}$-testosterone, $17{\alpha}$-testosterone), and gestagens (progesterone) and three synthetic hormones such as DES, zeranol, and taleranol. These hormones were analyzed by gas chromatographymass spectrometry. Newly developed multi-residue analysis method was applied for meat sample which were collected from market in the capital region and monitored the presence of residues of synthetic and natural steroid hormones. No residue of synthetic hormones were detected and endogenous level of progesterone was detected in cattle, pig and liver samples tested.

A comparative analysis of gas and liquid phase standard spiked solid sorbent tubes for the determination of volatile organic compounds in indoor air by TD-GC/MS (열탈착/저온농축-GC/MS에 의한 실내공기 중 휘발성 유기화합물 정량용 기체상 및 액체상 표준물질 첨가한 고체 흡착관의 비교 분석)

  • Lim, Hyun-Woo;Jung, Sung-Won;Kang, Chul-Ho;Park, Jin-Sook;Park, Byeong Moo;Choi, Yong-Wook
    • Analytical Science and Technology
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    • v.26 no.4
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    • pp.287-297
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    • 2013
  • The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

Determination of Liquid Paraffins in Foods by Using GC-FID (GC-FID를 이용한 식품 중 유동파라핀 함량 분석)

  • Park, Se-Jong;Choi, Jae-Chun;Lim, Ho-Soo;Jang, Su-Jin;Kim, So-Hee;Kim, Meehye
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.545-549
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    • 2013
  • Liquid paraffin is a mixture of heavier alkanes derived from petroleum. It can be used as a lubricant in processing machinery, as a coating agent, or as a releasing agent. The purpose of this study was to analyze liquid paraffins in foods by using a gas chromatography-flame ionized detector (GC-FID). Liquid paraffin was extracted from the food samples using n-hexane. Non-polar aromatic or olefinic co-extractives were removed by alkaline permanganate oxidation followed by clean up on an aluminium oxide SPE cartridge before the GC-FID analysis. The results of recovery tests were 91.5-103.2%. Based on this optimized method, we investigated the amount of liquid paraffin in various food samples purchased from domestic markets. The levels of liquid paraffin in bread were $95.5{\pm}156.0$ mg/kg (0.008%), those in capsules were $40.2{\pm}54.5$ mg/kg (0.001%), and those in dried fruits and vegetables were $3.0{\pm}18.1$ mg/kg (0.0001%). No liquid paraffin was detected in fresh fruits and vegetables. We propose that our method can be used to monitor and detect liquid paraffin in foods for food safety management.

Determination of Urinary Metabolite of Profenofos after Oral Administration and Dermal Application to Rats (흰쥐를 이용한 profenofos의 경구투여 및 피부도포 후 뇨 중 대사물질 측정)

  • 민경진;조영주;이인선;차춘근
    • Journal of Food Hygiene and Safety
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    • v.17 no.1
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    • pp.20-25
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    • 2002
  • This study was aimed to determine the urinary metabolite of profenofos, one of the organophos-phorus pesticides, as the biomarkers of exposure. Urine samples were collected fort 24 hours in metabolic cages after oral administration and dermal application of profenofos to rats. Identification of the derivatized urinary metabolite was determined by GC/MS and excretion time courses of the urinary metabolite was analyzed by GC/MS. Urinary metabolite of profenofos, 4-bromo-2-chlorophenol, was detected in rats urine both after oral administration and dermal application of profenofos. Parent compound was not detected in the experiment. In GC/MS, the mass spectral confirmation for 4-bromo-2-chlorophenol ion was identified at m/z 208.4-bromo-2-chlorophenol was excreted within 48 hours and 72 hours after oral administration and dermal application of profenofos, respectively. In this study, the same urinary metabolite of profenofos was detected both in oral and dermal exposure. Generally, excretion of the urinary metabolite after oral administration was detected faster than after dermal application. It is suggested that urinary 4-bromo-2-chlorophenol could be used as the biomarkers of exposure to profenofos.

Simultaneous determination of aromatic material causing allergic in children's products by Gas Chromatography (어린이 제품 중 가스 크로마토그래피를 이용한 알러지 유발 방향성 물질의 동시분석법)

  • Ko, Kyeong Mok;Rhu, Chan Joo;Kim, Jong Won;Lee, Seok Ki
    • Analytical Science and Technology
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    • v.31 no.1
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    • pp.23-30
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    • 2018
  • Twenty-two allergy-induced aromatics in children were analyzed using a gas chromatography flame ionization detector (GC-FID) and gas chromatography mass spectrometer (GC-MSD). Analytes were extracted using an automatic Soxhlet extractor and centrifuged for 10 min in a fast freezing centrifuge, and the supernatant was transferred into a 2 mL vial and injected in split mode. Under the established conditions, the calibration curve showed linearity with a correlation coefficient of 0.996 or more. A wide range of sensitivity of 6.7 to 1,859,839 depending on the device characteristics and detector used was shown. The detection limit of the device was 0.0032 to $0.0335{\mu}g/mL$, and the maximum detection limit was less than $0.1{\mu}g/mL$. The detection limit of the method ranged from 0.0033 to $0.1161{\mu}g/mL$. In addition, the limit of quantification ranged from 0.0100 to $0.5422{\mu}g/mL$, with a level of precision ranging from 0.21 % to 4.89 % and a degree of accuracy ranging from 89 % to 111 %. The analytical method developed in this study was applied to commercial products.