• Title/Summary/Keyword: GC method

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Dertermination of Alkylphenols, Chlorophenols and Bisphenol A in Various Samples by Freezing Filtration and GC/MS-SIM

  • Kim, Hyub
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.68.1-68.1
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    • 2003
  • A method for determination 11 endocrine disrupting chemicals of phenols in various samples was deloped. The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison; isobutoxycarbonyl (isoBOC) derivatization method and tert-butyldimethylsilyl (TBDMS) derivatization method. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then acetonitrile layer was refrigerated at -60$^{\circ}C$ for 2 hours (freezing filtration). (omitted)

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Volatile Flavor Components of Cultivated Radish (Raphanus sativus L.) Sprout (재배한 무순의 향미성분)

  • 송미란
    • The Korean Journal of Food And Nutrition
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    • v.14 no.1
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    • pp.20-27
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    • 2001
  • The consumption of radish ( Rhaphanus sativus L.) sprout, which is Cruciferae family, is increasing because of its pungent flavor and taste. Its volatile components were analyzed by SDE (simultaneous steam distillation & extraction) method and P&T(purge & cryogenic trapping) method. As a solvent, diethyl ether and diethyl ether : pentane mixture(2:1, v/v) were used in SDE method, and diethyl ether in P&T method. Analyzing by GC and GC-MS, the major component was sulfur compounds (19 species, peak area 76.6%) with diethyl ether, sulfur compounds(15. 44.0%) and hydrocarbons(23, 23.8%) with diethyl ether-pentane mixture in SDE method. Also, hydrocarbons(25, 84.1% ) was major component in P& T method. The major volatile component of fresh radish sprout were n-heptane, methyl pentane and that of boiled radish sprout were 4-methylthio-3-butenyl isothiocyanate, methyl mercaptane, 2,3-dimethyl disulfide. Low molecular volatile components were detected more by P& T method, but types and relative quantities of volatile components were measured less comparing to SDE method.

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Studies on Production and Efficient Utilization of Livestock Embryos by In Vitro Fertilization and Micromainipulation II. Effects of Embryonic Development on Survival after Freezing Transfer in Bovine Oocytes Fertilized In Vitro (체외수정 및 미세조작에 의한 가축(胚)의 생산과 효율적 이용에 관한 연구 II. 소 체외수정 난포란의 발생단계별 동결가 이식후의 생존성)

  • 정영채;김창근;윤종택;최선호;정광조
    • Korean Journal of Animal Reproduction
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    • v.17 no.3
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    • pp.233-242
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    • 1993
  • The effects of in vitro maturation and sperm treatment condition on the in vitro fertilization (IVF) and developmental capacity of bovine oocytes were investigated and the development of embryos was compared under the 2 different co-culture system, with GC or BOEC. The cultured embryo to 16 cell or morula wre transferred into recipients or frozen by 2 different freezing method. The results obtained were summarized as follows; 1. In vitro maturation rates of vovine follicular oocytes cultrued in TCM199 with 10% FCS or ECS were 64.0% and 72.7%, but the case of addition of 10% FCS or ECS to TCM199 co-cultured with granulosa cells were 81.3% and 84.0%, respectively. IVM rate of three TCM199 added to granulosa cells was higher than that of media without granulosa cells. 2. When bovine follicular oocytes were matured in TCM199 with 10% FCS and GC and then fertilized in vitro by sperm treated with caffeine, embryo developments of bovine oocytes co-cultured with BOEC were 38.4% and 51.4%, respectively. But those of bovine oocytes co-cultured with GC were 52.2% by sperm treated with caffeine-heparin. 3. Cleavage rates of bovine oocytes cultured with 10% FCS alone and fertilized in vitro by sperm treated with caffeine-heparin was 33.0%. 4. When bovine follicular oocytes were matured in TCM199 with 10% FCS and GC, embryo developments of bovine ooctyes co-cultured with BOEC of GC were 46.0% and 50.2%, respectively. 5. When bovine follicular oocytes were matured in TCM199 with 10% ECS and GC, embryo developments co-cultured with BOEC or GC were 45.2% and 51.4%, respectively. 6. When Korean Native cow's follicular oocytes matured in TCM199 with 10% FCS and GC, embryo developed co-cultured with BOEC or GC were 45.2% and 51.4%, respectively. 6. When Korean Native cow's follicular oocytes matured in TCM199 with 10% FCS and GC, embryo developments of the bovine oocyte co-cultured with BOEC and GC were 41.8% and 60.1%. But with FCS 10% those of the bovine oocytes co-cultured with BOEC and GC were 42.0% and 48.4%, respectively. 7. When Holstein's follicular oocytes were matured in TCM199 with 10% ECS and GC, embryo developments fo the bovine oocytes co-cultured with BOEC and GC were 50.0% and 57.7%, but with ECS 10% those of the bovine oocytes co-cultured with BOEC and GC were 52.2% and 56.5%, respectively. 8. The viability of frozen-thawed embryos ranged from 60~80% and those of frozen-thawed embryos from vitrification was lower than that from conventional metiod. 9. The selected fresh embryos were transferred nonsurgically to 7 recipients but did not result in pregnancy.

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Development of Fast Screening Method for Crop Protection Agents in Tobacco by Stir Bar Sorptive Extraction and Thermal Desorption coupled to GC/MS

  • Min, Hye-Jeong;Lee, Jeong-Min;Shin, Han-Jae;Lee, Moon-Yong;Jang, Gi-Chul
    • Journal of the Korean Society of Tobacco Science
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    • v.36 no.1
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    • pp.26-33
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    • 2014
  • Simultaneous determination of crop protection agents(CPAs) in food are done with multi-residue methods, which are composed of sample clean-up, concentration, chromatographic separation and detection. Stir Bar Sorptive Extraction(SBSE) technique is used for sample preparation of various analytes in several fields. The aim of this study was to develop a sensitive and fast method based on SBSE followed by thermal desorption - gas chromatography - mass spectrometry(TD - GC/MS) to determine CPAs in tobacco sample. For the analysis of tobacco sample prior to the SBSE method, solvent extraction or ultrasound-assisted solvent extraction was performed. methanol was used as the extraction solvent. The extract was then diluted with water. Finally, the sample was subjected to SBSE. A method for fast screening of crop protection agents in tobacco using SBSE-TD - GC/MS has been developed. About 17 CPAs including organochlorine, organophosphorous and others were identified and quantified. This method showed good linearity and high sensitivity for most of the target CPAs. The method was applied to the determination of CPAs at ng/mL levels in tobacco sample. This method is simple, rapid and may be applied in detection of other components.

Determination of Quintozene Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Quintozene의 잔류분석)

  • Ahn, Kyung-Geun;Kim, Gyeong-Ha;Kim, Gi-Ppeum;Hwang, Young-Sun;Hong, Seung-Beom;Lee, Young Deuk;Choung, Myoung-Gun
    • The Korean Journal of Pesticide Science
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    • v.19 no.3
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    • pp.195-203
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    • 2015
  • Quintozene, pentachloronitrobenzene (PCNB) is a contact fungicide for control of soilborne phytopathogenic fungi during cultivation of diverse crops. It was introduced to agricultural use around 1930's as a substitute for mercurial disinfectants. Although quintozene had been first registered in Korea on 1969. However, now it was banned to use due to its high residue levels in selected harvest products. Also, high possibility is expected that the residue may be contained in imported agricultural commodities as it is still used widely over the world. Therefore, this study was conducted to establish a determination method for quintozene residue in crops using GC/ECD/MS. Quintozene residue was extracted with acetonitrile from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and n-hexane partition was followed to recover quintozene from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The quintozene was quantitated by GLC with ECD, using a DB-1 capillary column. The crops were fortified with quintozene at 3 levels per crop. Mean recoveries ranged from 79.9% to 102.7% in five representative agricultural commodities. The coefficients of variation were less than 4.3%. Quantitative limit of quintozene was 0.004 mg/kg in representative five crop samples. A GC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of quintozene in agricultural commodities.

Derivatization and Residual Determination of MCPP in Soil Leachate (토양 침투수중 MCPP의 유도체화 및 잔류분석)

  • Hong, Moo-Ki;Smith, Albert E.
    • Korean Journal of Environmental Agriculture
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    • v.13 no.2
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    • pp.199-208
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    • 1994
  • Analytical methods for the determination of the derivatives of the herbicide (${\pm}$)-2-(4-chloro-2-methylphenoxy)propionic acid (MCPP) by capillary column gas chromatography with mass spectrometer (GC-MS) and electron-capture detection (GC-ECD) were studied. A successful procedure was introduced for the ester preparation using $H_2SO_4$, as the catalyst and the alcohol 2,2,2-trichloroethanol (TCE) or 2,2,2-trifluoroethanol (TFE). The identificaiton and elucidation of MCPP by GC-MS spectrometry following the esterification with diazomethane, $BF_3$/methanol, $H_2SO_4$/methanol, TCE, TFE, or pentafluorobenzyl bromide (PFB) were carried out. A comparison of the response-sensitivities among those MCPP esters was made with GC-ECD. Although the methylation product of MCPP was confirmed by GC-MS, its low sensitivity to the ECD limited the detection of MCPP. TCE, TFE, and PFB derivatization methods resulted in a high rate of MCPP esterifications and very sensitive ECD molecular responses. Based on efficiency, convenience, worker safety, and least sample contamination, TFE esterificaiton was considered as the superior method for MCPP analysis to the other methods of derivatization. An accurate method is described for quantifying MCPP in soil leachates by GC-ECD at very low concentrations without the requirement of a complicated clean-up process. As a result, MCPP residues at concentrations of less than $0.1{\mu}g$ in 100ml soil leachate were detected.

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Constructing Database for Drugs and its Application to Biological Sample by HPTLC and GC/MS (HPTLC와 GC/MS를 이용한 의약품의 데이타베이스화 및 생체시료에의 응용)

  • Yoo, Young-Chan;Park, Sung-Woo;Lim, Mie-Ae;Baeck, Seung-Kyung;Park, Seh-Youn;Lee, Ju-Seon;Lho, Dong-Seok
    • Analytical Science and Technology
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    • v.13 no.2
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    • pp.136-150
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    • 2000
  • For the identification of unknown drugs in biological samples, we attempted rapid high performance thin layer chromatographic method which is sensitive and selective chromatographic analysis of high performance thin layer chromatography (HPTLC) with automated TLC sampler and ultra-violet (UV) scanner. We constructed HPTLC database (DB) on two hundred five drugs by using the data of Rf values and UV spectra (scan 200-360 nm) as well as gas chromatography/mass spectrometry (GC/MS) DB on ninety six drugs by using the data of relative retention time (RRT) on lidocain and mass spectra. After extracting drugs in biological sample by solid phase extraction (Clean Screen ZSDAU020), we applied them to HPTLC and GC/MS DB. Drugs, especially extracted from biological samples, showed good matching ratio to HPTLC DB and these drugs were confirmed by GC/MS. In conclusion, this DB system is thought to be very useful method for the screening of unknown drugs in biological samples.

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Studies on Pretreatment for Analysis of Pesticides by Using HPLC and GC (HPLC 및 GC에 의한 농약분석에서 전처리에 대한 연구)

  • Oh, Bo Young;Bae, Jun Hyun;Kang, Jun Gil;Kim, Youn Doo
    • Journal of the Korean Chemical Society
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    • v.43 no.6
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    • pp.663-669
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    • 1999
  • For determination of separated pesticides by using GC and HPLC, liquid-liquid extraction(LLE) and solid phase extraction(SPE) have been carried out to separate and concentrate the organophophorous pesticides such as Diazinon, Fenitrothion, Phosmet, Phosalon and EPN in environmental water samples. ln determination of pesticides by HPLC/UV, SPE has resulted in higher recovery and more precision than LLE, while in determination of pesticides by GC/FPD, vice versa. HPLC/UV after the pretreatment process of sample by solid phase extraction (SPE-HPLC/UV) has suggested the possibility of determination of pesticides ppb level. ln comparison of detection limit, both SPE-HPLC/UV and LLE-GC/FPD are reasonably suitable for analysis of residue pesticides. ln the respect of the rapidity and the solvent required, SPE-HPLC/UV method has proven to be superior to LLE-GC/FPD.

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Determination of Nicotine and Other Minor Alkaloids in Tobacco Leaves by GC/MS (GC/MS를 이용한 잎담배 중 알칼로이드 함량 분석)

  • Lee Jeong-Min;Min Hye-Jung;Kim Yong-Ha;Rhee Moon-Soo
    • Journal of the Korean Society of Tobacco Science
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    • v.27 no.1 s.53
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    • pp.100-106
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    • 2005
  • To obtain the optimum condition for analysis of 10 alkaloids in tobacco leaves, such as nicotine, nornicotine, anatabine, anabasine, myosmine, cotinine, 2,3'-dipyridyl, $\beta-nicotyrine,\;\beta-nornicotyrine\;and\;\beta-formylnornicotin$, 5 types of extraction method were investigated by GC-FID and GC/MS. The optimum condition of alkaloid extraction was achieved by using methanol:dichloromethane(1:3, v/v) after NaOH treatment. The use of mass selective detector (MSD) provided unambiguous nicotine related alkaloid analysis. Alkaloids in various tobacco leaves were extracted with the optimum extraction condition and quantified by GC/MS/SIM mode. Compared with concentrations of alkaloids among the various tobacco leaves, the concentration of alkaloids was generally in the order burley > flue-cured > oriental tobacco. In flue-cured tobacco leaves, the order of concentration of alkaloids was nicotine > anatabine > nornicotine > $\beta-nicotyrine\;>\;\beta-formylnornicotine\; >\;myosmine\;>\;2,3'-dipyridyl\;>\;cotinine\;>\;anabasine\;>\;\beta-nornicotyrine$. However, in the case of burley and oriental tobacco leaves, the concentration of nornicotine was higher than that of anatabine.