• Title/Summary/Keyword: GC-MS (SIM)

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Analysis of Benzene in Beverages by Headspace-GC/MS (Headspace-GC/MS를 이용한 음료 중 벤젠 분석)

  • Kim, Eun-Ju;Park, Sang-Aeh;Choi, Dong-Mi
    • Journal of Food Hygiene and Safety
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    • v.22 no.4
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    • pp.243-247
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    • 2007
  • A selective analytical method of headspace-GC/MS has been applied to determine levels of benzene in beverages. Food samples were 85 including 2 fruit juices, 6 fruit beverages, 11 carbonated beverages, 55 mixed beverages, and 4 beverage concentrations, and 7 extracted beverages. For phase equilibration of headspace, sample was stirred at $40^{\circ}C$ for 30 min. The oven temperature was $60^{\circ}C$ and elevated to $180^{\circ}C$ at $15^{\circ}C/min$. The internal standard was benzene-d6. The identification was done by the selected target ions such as m/z 51, 77, and 78 and the confirmation was done by the response ratio of m/z 77 to m/z 78 between sample and standard. The overall recoveries were ranged from 91% to 101% and the limit of quantification was $1{\mu}g/kg$. The average level of benzene were $5{\mu}g/kg$ for fruit beverages, $2{\mu}g/kg$ for carbonated beverages, $7{\mu}g/kg$ for mixed beverages and $7{\mu}g/kg$ for extracted beverages.

Monitoring of Butyltin Compounds in PVC Food Packaging - Determination of Butyltin Compounds in PVC Wrap and Gasket for Food Packaging by GC/MS (식품용 염화비닐수지제 기구 및 용기.포장 중 부틸주석화합물의 모니터링 - GC/MS를 이용한 염화비닐수지제 식품용 랩 및 가스킷 재질 중 부틸주석화합물 잔류량 분석)

  • Sung, Jun-Hyun;Yoon, Hae-Jung;Choi, Hyun-Cheol;Jeon, Dae-Hoon;Eom, Mi-Ok;Kim, Hyung-Il;Park, Na-Young;Lee, Eun-Joon;Lee, Young-Ja
    • Korean Journal of Food Science and Technology
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    • v.39 no.6
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    • pp.715-720
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    • 2007
  • The levels of butyltin compounds in poly(vinyl chloride) (PVC) food packaging using gas chromatography/mass spectrometry (GC/MS) were monitored. The analytical method, involving the ethylation with sodium tetraethylborate, was found to be selective and sensitive for mono-n-butyltin (MBT), di-n-butyltin (DBT), and tri-n-butyltin (TBT), validated by a $0.005\;{\mu}g/mL$ limit of detection (LOD), an $R^2>0.999$ for linearity, and >90% of recovery, respectively. Finally, none of the commercial food wraps and gaskets showed detectable levels of butyltin compounds.

Analysis of Thiosultap in Hulled Rice by Derivatization (유도체화 반응에 의한 현미 중 thiosultap의 분석)

  • Choi, Jeong-Heui;Do, Jung-Ah;Yoon, Hae-Jung;Park, Yong-Chun;Kim, Jae-Hun;Choi, Dong-Mi
    • The Korean Journal of Pesticide Science
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    • v.14 no.1
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    • pp.16-20
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    • 2010
  • Thiosultap, a nereistoxin analog insecticide, registered in China has been used to control selected beetles and Lepidopteran pests on rice, vegetables and fruit trees. Although domestic use of thiosultap is not permitted, it is needed to monitor this insecticide from imported crops because that has been used on crops in many foreign countries, especially China. Thiosultap in hulled rice was determined as nereistoxin derived in basic condition by GC-FPD. This method accomplished ion-associated liquid-liquid partitioning for cleanup, and limit of quantification and linearity performed by the established method were 0.05 mg $kg^{-1}$ and 0.995$(r^2)$. The recoveries performed by control hulled rice fortified with thiosultap at 0.5 and 2.5 mg $kg^{-1}$ were $96.1{\pm}7.9\sim100.8{\pm}6.1%$.

Analytical Method of Epichlorohydrin in Canned Beverages by Purge-and- Trap/GC

  • Lee Kwang-Ho;Kwak In-Shin;Kim Dyoung-Il;Choi Byoung-Hee;Kim Guy-Joung;Lee Chul-Won
    • Proceedings of the Korean Society of Food Hygiene and Safety Conference
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    • 2001.10a
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    • pp.140-140
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    • 2001
  • A sensitive analytical method based on gas chromatograpy-mass spectrometry with a selected ion monitoring (GC/MS-SIM) with the purge-and-trap concentration and with headspace method (in limited applications) was developed for determining of epichlorohydrin in canned beverages coated with epoxy resin. The calibration curve in the range of $0.5\sim50ng$ had correlation coefficient greater than 0.998 and a detection limit of $0.l\mug/L$ was obtained using a sample volume of 20ml. The predominant ions of epichlorohydrin produced in MSD using electron ionization(EI) were m/z 57 ([M-CI]+) and 62/64 $([M-CH_2O]+)$. In survey of epichlorohydrin in thirty commercial canned beverage samples, none of them was detected.

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Simultaneous Analysis of Pesticide Priority Pollutants in Water Samples (수질 시료 중의 Pesticide Priority Pollutants 동시분석에 관한 연구)

  • Kim Kye-Young;Kim Chong-Hyeak;Lee Sueg-Geun
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.590-598
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    • 1993
  • The simultaneous analysis of samples, 16 organic pesticides in water among 129 priority pollutants listed by EPA, was performed by GC-ECD (electron capture detector) and GC/MS-SIM (selected ion monitoring). Two extraction procedures, liquid-liquid extraction (LLE) and solid-phase extraction (SPE), were studied as an extraction and concentration method. Accuracy and precision of the methods were measured by the calculation of mean recovery and mean relative standard deviation. Finally, the detection limits, the experimental limitations, and prospects were discussed.

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Gibberellins Production and Identification of Endophytic Fungi Isolated from Aquatic Plant in Fresh Water (담수에 자생하는 수생식물에서 분리된 내생균류의 지베렐린 생산과 동정)

  • You, Young-Hyun;Kang, Sang-Mo;Choi, Yu-Mi;Lee, Myung-Chul;Kim, Jong-Guk
    • The Korean Journal of Mycology
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    • v.43 no.1
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    • pp.71-76
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    • 2015
  • Aquatic plant Hydrocharis dubia (Blume) Backer was collected from the Dalsung wetland in Daegu. Sixteen endophytic fungi with different colony morphologies were isolated from the roots of aquatic plants. Waito-c rice (WR) seedlings were treated with fungal culture filtrates (FCF) for screening plant growth-promoting activity. In the results, HD1008 strain isolated from aquatic plant showed highest plant growth-promoting activity. The FCF of HD1008 strain was analyzed using gas chromatography mass spectrometry (GC/MS) with selected ion monitoring (SIM). Analysis of the FCF of HD1008 strain found that it contained gibberellins (GA) ($GA_1$, 1.2 ng/100 mL; $GA_4$, 5 ng/100 mL). Phylogenetic tree of HD1008 strain was constructed by partial internal transcribed spacer (ITS) region and partial beta-tubulin gene sequences. Therefore, we describe HD1008 strain as a new gibberellin-producing Penicillium trzebinskii based on morphological and molecular characteristics.

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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Dependence of Ethyl Carbamate Formation on the Fermentation Variables in Korean Traditional Soysauce (재래식 간장의 제조조건이 ethyl carbamate 생성에 미치는 영향)

  • 정현정;권훈정
    • Korean journal of food and cookery science
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    • v.13 no.2
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    • pp.92-98
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    • 1997
  • Ethyl carbamate is an animal carcinogen and a by-product of fermentation. Since the highest level of ethyl carbamate was found in a traditional soy sauce sample in the previous study, soysauce was prepared in varying experimental conditions with three kinds of meju originated from different area of the country to investigate the factors affecting ethyl carbamate formation. The sample analysis methods included a semi-purification with solid-phase extraction and detection by GC-MS at SIM mode using m/z 62 fragment ion. Among the investigated factors, which includes source meju, bringing length, salt content, irradiation of visible light during bringing or storage, and storage length, source meju and storage length showed most profound effect on the formation of ethyl carbamate. Irradiation of visible light for 12 hours a day during storage lowered the concentration of ethyl carbamate compared to the soysauce kept in the dark. Meanwhile irradiation during the bringing as well as the degree of salt contents showed no effect.

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Analysis for 16 Polynuclear Aromatic Hydrocarbons (PAH) in Sewage Sludge and Soil (하수슬러지와 토양 중 다핵방향족 탄화수소의 정량)

  • Kim, Jong-Hun
    • Analytical Science and Technology
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    • v.13 no.3
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    • pp.357-367
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    • 2000
  • The polycyclic aromatic hydrocarbon (PAH) content in sewage sludge and in farm soils were determined by gas chromatography linked to mass spectrometry (GC/MS) with use 2-ethylantracene as internal standards. Twelve PAH were identified in both sludges with naphthalene ($0.78{\mu}g/g$) being the most predominant in industrial sludge and pyrene ($0.26{\mu}g/g$) in municipal sludge. The total PAR content in industrial sludge and in municipal sludge were $1.74{\mu}g/g$ and $1.19{\mu}g/g$ respectively. PAH were contained in paddy soils and the concentration were very low in the range of $0.01-0.04{\mu}g/g$. The total PAH content in industrial and in municipal sludge were about 9.2 times and 6.3 times greater than in paddy soils ($0.19{\mu}g/g$).

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Diurnal Variation in Endogenous Gibberellin Levels of Rice Shoots

  • Hwang, Sun-Joo;Hamayun, Muhammad;Kim, Ho-Youn;Kim, Kil-Ung;Shin, Dong-Hyun;Kim, Jang-Eok;Kim, Sang-Yeol;Lee, In-Jung
    • Journal of Crop Science and Biotechnology
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    • v.10 no.3
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    • pp.163-166
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    • 2007
  • Diurnal changes in levels of endogenous gibberellins(GAs) were investigated in three rice cultivars i.e. Sangjubyeo, Shingeumobyeo(photo-neutral) and Chucheongbyeo(photosensitive). The rice cultivars were grown under a 12-hr photoperiod and endogenous GA levels were assayed by gas chromatography-mass spectrometry(GC-MS-SIM) every 3 h for 24 h. The endogenous bioactive $GA_1$ and its immediate precursor $GA_{20}$ contents were significantly different in both photosensitive and photo-neutral rice cultivars, though less pronounced differences were observed for endogenous $GA_{12},\;GA_{53},\;GA_{19}$, and $GA_8$ levels with in the three rice cultivars. The levels of bioactive $GA_1$ and its immediate precursor $GA_{20}$ were significantly higher in Chucheongbyeo than in the other two cultivars. In Chucheongbyeo, the $GA_1$ contents increased significantly from 11.00 to 17.00 o'clock, thus indicating a correlation with light. In Shingeumobyeo, $GA_1$ contents slightly increased during morning hours, while a similar hike in $GA_1$ contents was observed for Sangjubyeo during evening hours. $GA_{19}$ was found to be the most abundant GA form in the three rice cultivars. Our results suggested that GA production in rice depends upon the response potential of rice cultivars and that light positively correlated to GA production in photosensitive rice cultivar.

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