• 농약과학회지
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• 제19권4호
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• pp.345-353
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• 2015

본 연구는 GC/NPD와 GC/MS를 이용하여 농산물 시료에 적용 가능한 MBI propionamide계 살균제 fenoxanil의 잔류 분석법을 확립하였다. 고추, 배추, 사과, 현미 및 콩을 대표 농산물로 설정하여 fenoxanil 단성분의 정량 및 확인 시험법을 개발하였다. 각각 농산물에 대한 추출은 acetone을 이용하였으며, 분배과정은 n-hexane/dichloromethane (80/20, v/v), 정제는 florisil 흡착제를 활용한 정제법을 적용하였다. 정량분석은 DB-5 capillary column을 GC/NPD에 장착하여 수행하였고, 각 농산물에 대한 정량한계는 0.04 mg/kg으로 설정 가능하였다. 회수율은 82.2-109.1%로 조사되었으며 농산물 시료의 종류 및 처리수준에 관계없이 7.2% 미만의 변동계수를 나타냈다. 정성적 확인을 위해 GC/MS를 이용, m/z 125.0, 188.9 및 293.0을 fenoxanil의 정성확인을 위한 선택적 이온으로 설정하였다.

• 원예과학기술지
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• 제34권1호
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• pp.183-194
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• 2016

본 연구는 국내 및 수출입 원예작물의 일상적 잔류농약 검사에 활용 가능한 dinitroaniline계 광범위 살균제 fluazinam의 GC-ECD/MS 잔류 분석법을 확립하고자 하였다. 원예작물 중 채소류에서는 청양고추와 결구배추를, 과일류에서는 감귤과 사과를 대표 시료로 선정하였고, 아세톤으로 추출된 fluazinam은 식염수로 희석하고, 수용액층을 n-hexane 액-액 분배법으로 회수하였으며, 회수된 추출액으로부터 fluazinam의 최종적 정제를 위하여 florisil 칼럼 크로마토그래피법으로 추가 정제하여 GC-ECD/MS 분석용 시료로 사용하였다. Fluazinam의 정량적 분석을 위하여 DB-17 capillary column을 적용한 GC-ECD 분석 조건을 확립하였으며, 각 작물별 4수준의 농도로 fluazinam을 인위 첨가하여 회수율을 분석하였다. 각 대표 원예작물에 대해 정량한계, 정량한계의 10, 50, 및 100배 수준에서 회수율을 검토한 결과 모든 처리농도에서 82.5-99.9% 수준을 나타내었으며, 정량한계(LOQ)는 $0.004mg{\cdot}kg^{-1}$이었다. 반복 간 변이계수(CV)는 최대 6.6%를 나타내어 국제적 잔류분석 기준인 회수율 70-120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였다. 또한 GC/MS SIM을 이용하여 실제 각 작물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 fluazinam의 GC-ECD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로서 국내 및 수출입 검역을 위한 원예작물의 공정 잔류분석법으로 사용 가능할 것이다.

• 대한화장품학회지
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• 제22권2호
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• pp.153-160
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• 1996

A novel simple method to detect vitamins in cosmetic products by gas chromatography-mass spectrometry(GC-MS) has been developed. Three vitamins(panthenol, cholecalciferol and tocopherol) were used for this study. Vitamins were prepared by dissolving in tetrahydrofuran(THF), and silylated with bis-trimethylsilyltrifluoroacetamide-trichloromethylsilane(BSTFA). Silated vitamins were separated on a fuses-silica capillary column coated with DB-5. The identification of each vitamin was accomplished by retention time and mass spectrum library search with a computer, and the quantitation was made in the selected-ion monitoring(SIM) mode of GC-MS. SIM mode had given sensitivity to determine 50pg of panthenol, 285pg of cholecalciferol and 130pg of tocopherol. Linearity was maintained over the range 0.005-0.20% for each vitamin. Each cosmetic product(i.e. hair tonic and lotion) was found to contain amounts of the vitamins. This method was sensitive and gave 77.5-99.9% recovery of each vitamin from these cosmetic products. From these results, we concluded that silylation with BSTFA followed by GC-MS analysis allows the simple, covenient and exact determination of panthenol, cholecalciferol and tocopherol.

• Toxicological Research
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• 제25권1호
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• pp.41-45
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• 2009

This study was conducted to monitor the level of bifenthrin residues in pear sprayed with 2% bifenthrin wettable powder (WP) at the recommended rate at four different schedules prior to harvest. The target analyte was extracted with acetone, partitioned into dichloromethane, and then purified by florisil chromatographic column. The residue determination was performed on a DB-5 capillary column using GC with electron capture detector (ECD). Linearity of this method was quite good ($r^2$ = 0.9951) in the concentration ranged from 0.2 mg/kg to 10 mg/kg. Recovery test was carried out at two concentration levels, 0.2 mg/kg and 1.0 mg/kg, in three replicates, and their rates were from 82.9% to 107.2%. No quantitative bifenthrin was detected in pear of all kinds of treatments including the treatment sprayed 4 times until 7 days before harvest. This sensitive and selective method can be used to monitor the trace residual amounts of bifenthrin in pear in a quite low concentration level.

• 분석과학
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• 제26권5호
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• pp.315-325
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• 2013

The possibility of acute hepatotoxicity caused by dimethylformamide (DMF) requires regular monitoring of the workers who are using DMF to prevent the occupational disease. The authors performed ambient and biological monitoring of workers involved in synthetic leather manufacturing processes using DMF to assess the correlation between the markers of ambient and biological monitoring of DMF. The authors monitored 142 workers occupationally exposed to DMF from 19 workshops in the synthetic leather and ink manufacturing industries located in northern region of Gyeonggi-do. The subjects answered questionnaire on work procedure and use of personal protective equipment to be classified by exposure type. DMF in air samples collected using personal air samplers, diffusive and active sampler, was analysed using gas chromatograph-flame ionization detector (GC-FID) with DB-FFAP column (length 30 m, i.d. 0.25 mm, film thickness 0.25 ${\mu}m$). Urinary N-methylformamide (NMF) was analysed using gas chromatograph-mass selective detector (GC-MSD) at selected ion monitoring (SIM) mode with DB-624 column (length 60 m, i.d. 0.25 mm, film thickness 1.40 ${\mu}m$). Geometric mean (GM) and geometric standard deviation (GSD) of the ambient DMF was $6.85{\pm}3.43$ ppm, and GM and GSD of urinary NMF was $42.3{\pm}2.7$ mg/L. The ratio of subjects with DMF level over 10 ppm was 44%, and those with urinary NMF over 15 mg/L was 87%. NMF in urine adjusted by DMF in air was $4.61{\pm}2.57$ mg/L/ppm and $9.50{\pm}2.41$ mg/L/ppm, respectively, with or without respirator. There was seasonal differences of NMF in urine adjusted by DMF in air, $7.63{\pm}2.74$ mg/L/ppm in summer and $4.53{\pm}2.29$ mg/L/ppm in winter. The urinary NMF concentration which corresponds to 10 ppm of ambient DMF was 52.7 mg/L (r=0.650, n=128). Considering the difference of the route of exposure which resulted from the compliance of wearing personal protective equipment, the estimated contribution of respiratory and dermal exposure route for DMF was 48.5% vs. 51.5%.

• 분석과학
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• 제27권6호
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• pp.339-346
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• 2014

근로자 건강진단 실무지침 상의 필수 검사항목 항목 중, N-메틸아세트아미드의 소변 표준시료를 제조하여 그 신뢰도를 확인하고자 하였다. DB-624 컬럼을 사용한 GC/MSD 분석 방법에 의해 기존 분석 컬럼보다 우수한 분리능과 선택성으로 N-메틸아세트아미드를 분석하였다. -60, -20, 5, $25^{\circ}C$에서 5-50 mg/L의 농도 범위의 소변 중 N-메틸아세트아미드의 안정성을 6개월 보관 시점까지 검토한 결과 모든 보관 조건에서 안정하였으며, 각 시료에 대한 균질성 검사 결과도 양호하였다. 이상의 결과로부터 유리형 NMAC를 첨가하는 방법으로 제조한 소변 중 NMAC 표준시료가 분석정도관리용으로 실용화하기에 적합한 균질성과 장기간 보관 시의 안정성을 모두 만족시킴을 확인하였고, 2008년부터 분석정도관리 표준시료로 활용하였다.

• Archives of Pharmacal Research
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• 제27권5호
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• pp.539-543
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• 2004

An efficient analytical method was devised for the accurate L-muscone assay in aqueous samples. It involves solid-phase extraction of L-muscone in adsorption mode using XAD-4 as the sorbent and dichloromethane modified with 10% (v/v) methanol as the eluting solvent. The gas chromatographic analysis of the eluate residue dissolved in toluene on a DB-5MS capillary column provided complete resolution of L-muscone from the co-extracted interferences. The overall method showed excellent linearity ($r^2{\geq}$ 0.9994) in the range of 0.1 to 2.0 $\mu\textrm{g}$/mL with good intra- and inter-day precisions (% RSD = 2.5～7.3) and with high extraction recovery rates ($\geq$ 98.1 %). When the present method was applied to a L-muscone herbal drink product, the within-batch RE (%) in the labeled concentration (1.5 $\mu\textrm{g}$/mL) for the three randomly chosen bottles were -2.4, -1.3 and -3.3 with high precision (% RSD $\leq$ 3.1). The present method is considered to be suitable for quality control evaluation on liquid drinks and other complex formulations fortified with L-muscone.

• 한국식품과학회지
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• 제26권2호
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• pp.162-166
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• 1994

Gas chromatography를 이용한 profiling과 신속한 동정을 여러 알코올 음료(적포도주, 백포도주, 맥주, 브랜디)속에 존재하는 휘발성 및 비휘발성 유기산의 동시분석에 적용하여 보았다. 흡착제로 Chromorb P와 용출용매로 diethyl ethe를 사용하는 고체상추출법을 이용하여 알코올 음료로부터 유기산을 분리한 후, triethylammonium염으로 만들었다. 그 후 유기산을 tert.-butyldimethylsilyl 유도체로 만들어 극성이 다른 DB-5와 DB-1701 두 컬럼으로 동시분석하였다. 두 컬럼에서 분리된 유기산 피크들을 dual capillary column system의 retention index (RI) library 탐색과 면적비(AR) 비교로 신속하고 정확하게 동정할 수 있었으며 이들을 GC-MS로 확인하였다. 알코올 음료들의 유기산 분석결과, fatty acid, dioc acid, hydroxy acid, aromatic acid 등 29가지의 유기산이 동정되었고 각 음료의 증류에 따라 특징적인 유기산 GC profile을 나타내었다. 각 음료의 GC profile의 유기산 조성만을 단순화시킨 RI spectra로 표현한 결과, 각 음료의 유기산 패턴의 분별이 매우 용이하였으며, Direct comparison법을 시도해 본 결과, 998 ppt의 match quality값을 나타내어 임의의 시료가 적포도주임을 알 수 있었다.

• 약학회지
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• 제41권3호
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• pp.277-282
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• 1997

Methamphetamine, which is the most commonly abused drug in Korea, exists in terms of d-, l- isomers and a racemate(dl). d-Methamphetamine is a potent central nervous system stimulant, whereas l-Methamphetamine is sold freely as a nasal decongestant. In addition, methamphetamine appears in different ratios of optical isomers by the clandestine synthesis applied. In this study, enetiomeric separation of methamphetamines was estabilished to distinguish the chirality of methamphetamines trafficked and abused in Korea. A gas chromatograph/mass spectrometer(GC/MS) system equipped with an achiral capillary column is used to isolate the isomers of methamphetamine after (S)-N-(trifluoroacetyl)-l-prolyl(TFP) deravatization.After analyzing 10 illicit methamphetamine powders and 10 positive urine samples, following findings were found: d-Methamphetamine was well resolved from l-Methamphetamine by chromatographic separation of TFP derivatibes on DB-5 with retention time of 11.80 and 11.35 min respectively. The detection of d-Methamphetamine in all 10 powders and 10 urine samples proves that all methamphetamines abused in Korea are illegally manyfactured and administred.

• 한국연초학회지
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• 제14권1호
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• pp.66-78
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• 1992

The essential oil of Korean valerian root ( Valeriana fauriei roar. dasycarpa Hara) was isolated by simultaneous distillation Sl extraction. The oil content of fresh root was 0.7% (wb) and that of dried root was 2.1 5 (db) and sensory analysis of the oil indicated sweet-balsamic, woody and floral characteristic aroma notes. The oil was fractionated into one hydrocarbon fraction and three oxygenated hydrocarbon fractions by using silica gel column chromatograpy. Each fraction was analyzed by capillary GC and GC-MS. Out of 81 characterized compounds, the major compounds were a-pinene, camphene, $\beta$-pinene, bornyl acetate, borneol , bornyl iso-valerate and sesquiphellandrene and the characteristic floral and woody aroma of neutral fraction of Korean valerian root could be due to be the presence of oxygenated compounds such as borneol, bornyl acetate, bornyl iso-valerate, p-ionone ana $\beta$-ionone epoxide. Comparing the yield of Korean valerian root with those from other origins reported, oil content of Korean valerian root was higher than those of European and Indian origins.