• 한국환경농학회지
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• 제34권4호
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• pp.309-317
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• 2015

본 연구는 GC-ECD/MS법을 적용하여 농산물에 함유된 phenylpyrazole 살충제 fipronil의 잔류 분석법을 확립하였다. 대표 농산물은 사과, 고추, 배추, 현미 및 콩을 선정하였고, acetone에 의해 추출된 fipronil 성분을 n-hexane/dichloromethane 액-액 분배법과 florisil 흡착크로마토그래피법으로 정제하여 분석시료로 사용하였다. Fipronil의 정량적 분석을 위한 최적 GC-ECD 분석 조건을 확립하였으며 정량한계(LOQ)는 0.004 mg/kg이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과, 모든 처리농도에서 86.6-106.0% 수준을 나타내었고, 반복 간 변이계수(CV)는 최대 5.7%를 나타내어 잔류분석 기준인 회수율 70-120% 및 분석오차 10% 이내를 충족시키는 결과를 도출하였으며, GC/MS/SIM을 이용하여 실제 농산물 시료에 적용하여 재확인하였다. 이상의 결과로 신규 fipronil의 GC-ECD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

• Food Quality and Culture
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• 제1권1호
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• pp.13-17
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• 2007

The volatile flavor compounds of Saussurea lappa C.B. Clarke, a perennial, aromatic and medicinal herbaceous plant of the Asteraceae family, were isolated by the hydro distillation extraction method using a Clevenger-type apparatus, and analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC/MS). The plant yielded a light yellow colored oil (0.02%, v/w). From S. lappa C.B. Clarke root oil, sixty-three volatile flavor compounds were tentatively identified, among which sesquiterpene was predominant (21.70%). The identified compounds of the root oil constituted 87.47% of the total peak area. From the constituents making up more than 5% of the volatile flavor components, a long-chain aldehyde, (7Z, 10Z, 13Z)-7, 10, 13-hexadecatrienal, was the most abundant volatile flavor compound (21.20%), followed by dehydrocostuslactone (10.30%) belonging to sesquiterpene lactone, valerenol (5.30%) and vulgarol B (5.06%).

• 한국산업보건학회지
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• 제11권3호
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• pp.206-211
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• 2001

This article describes identification and quantification of benzene in the casting process. Air samples around the casting process were taken by using personal air sampler attached charcoal tube and desorbed by carbon disulfide. The identification and quantitative analysis of benzene have been performed by GC-MS and GC-FID. Calibration range of standard solutions for benzene was prepared in range from 0.1 to 2 times of TLVs concentrations($1.4{\sim}28{\mu}g/1m{\ell}$ CS2) and the limit of detection was $0.11{\pm}0.002{\mu}g/1m{\ell}$ CS2. Benzene detected in airborne was ranged in 4.0ppb~104.7ppb.

• 농업과학연구
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• 제36권2호
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• pp.219-224
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• 2009

효소적 공법을 이용하여 합성한 기능성 modified-butterfat들(MF668과 MF866)의 향기성분 분석을 전자코와 SPME-GC/MS를 가지고 수행하였다. 전자코 분석결과, 기질로 사용된 ABF와 FSO, 그리고 생성물인 MF668과 MF866은 제1주성분 값의 95.16%기여율로 서로 다른 향기패턴을 갖음을 확인하였다. 신속하며 간편한 SPME-GC/MS분석결과, MF668과 MF866에서는 기질에서보다 더 다양한 aldehyde류, ketone류, acid류 등이 검출되었다. 이는 반응과정 중 생성될 수 있는 산화물로 추후 항산화제 연구가 필요함을 입증하였다.

• 농업과학연구
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• 제43권4호
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• pp.634-640
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• 2016

The objective of this study was to evaluate the effectiveness of using HR-GC/MS for the rapid screening of dieldrin residues in soils. Persistent organic pollutants (POPs) of organochlorine pesticides such as dieldrin, were analyzed in sedimentary rock and granite rock collected from greenhouses, Niigata, Japan. Dieldrin remains in Japanese farming soils, more than 40 years after their use as insecticides was prohibited. The averages in soil moisture ranged from 2.79% to 7.20% in soils derived from sedimentary rock and from 25.59% to 31.40% in soils derived from granite rock. Mean concentrations of dieldrin residues in sedimentary rock and granite rock were $39.7ng\;g^{-1}$ and $40.51ng\;g^{-1}$, respectively. Dieldrin residue was detected at a slightly higher concentration in granite rock than sedimentary rock samples. There was no consistency between the two soils or between surface and subsurface soils. The coefficients of variation of the two soils were 10.6% and 8.7%, respectively. These results suggest that our high-resolution mass spectrometry detector (HR-GC/MS) is effective at analyzing residual organochlorine pesticides in soil. In order to increase the precision and sensitivity for chemical analysis of POPs, high-resolution gas chromatography coupled with a HR-GC/MS is highly recommended.

• 분석과학
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• 제14권2호
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• pp.109-114
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• 2001

담배에 포함된 향료 성분을 headspace solid phase microextraction(SPME)를 이용하여 gas chromatography-mass spectrometry(GC-MS)의 selected ion monitoring(SIM)방법으로 분석하였다. 본 연구에서 사용한 담배향과 관련된 성분은 estragole, pulegone, trans-anethole, safrole, piperonal, eugenol, methyleugenol, coumarin, trans-isoeugenol, trans-methylisoeugenol 및 myristicin 등 11종이며 분석결과 모든 담배에서 한가지 또는 그 이상의 담배향 성분을 $0.001-1.3{\mu}g/g$ 검출할 수 있었으며 회수율은 89.1-102.9%로 나타났고 상대표준편차는 2.6-25.2%를 얻었다.

• Mass Spectrometry Letters
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• 제3권1호
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• pp.15-17
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• 2012

Eighteen of the PDE-5 inhibitors and their analogues were analyzed using GC-EI-MS. Fourteen of them could be identified by simple GC-MS method without derivatization, but hydroxyhongdenafil, hydroxyvardenafil, xanthoanthrafil and mirodenafil could not be identified without derivatization for the high polarity due to the presence of hydroxyl groups. N,O-bis(trimethylsilyl) trifluoroacetamide (BSTFA) and N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), widely used trimethylsilyl (TMS) derivatizing reagents, were used to improve the sensitivity of the hydroxylated analogues. And the analytes could be identified by GC-MS after the derivatization.

• 복식문화연구
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• 제12권4호
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• pp.579-590
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• 2004

This research was aimed to investigate and compare the effectiveness of TLC and GC-MS methods in the analysis of chromophoric substances extracted from madder plant. Alizarin and purpurin 0.3% solution were used as comparative standards; madder extraction was prepared by heating the solution of powdered madder at 80℃, pH 1.5, for 90 min. Best elution solvent for TLC in silica gel plate was toluene:ethyl acetate=9:1, which resulted in red and yellow spots from madder extraction each of which showed R/sub f/ values 0.32-0.43 and 0.07-0.11. Although the red spot in particular exhibited similar characteristics as standard purpurin in color, shape, and R/sub f/ values, the result was inconsistent throughout different TLC trials. GC-MS analysis showed only small amount of alizarin and no purpurin in the madder extraction. Other chromophoric substance such as 2-furancarboxaldehyde, 5-(hydroxymethyl)-, anthralin, and danthron were also detected in small amounts. The result indicated that TLC was less sensitive to detecting and identifying the natural dyestuff which is generally constituted with a number of similar but chemically different chromophoric substances.

• 분석과학
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• 제18권6호
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• pp.453-459
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• 2005

물중에 존재하는 11종의 페놀류를 benzoyl chloride를 사용하여 물에서 직접 유도체화한 후 추출하여 동시 분석하였다. 즉, 수용액 시료에 수산화나트륨 용액을 가하여 pH 13으로 조절한 다음 여기에 benzoyl chloride를 $500{\mu}L$을 가하여 15분간 흔들어 반응시키고 정치한 후 diethyl ether로 추출하여 GC/MS-SIM으로 정량하였다. 검량선은 $0.05-5.0{\mu}g/mL$ 농도범위에서 상관계수가 $r^2=0.9915$로 직선성이 좋았으며 상대표준편차는 8.5% 이하였고 이 방법의 회수율은 58.4-114.0% 이었다.

• Mass Spectrometry Letters
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• 제15권2호
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• pp.79 -94
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• 2024

Over the past few decades, new psychoactive substances (NPS) have become prevailing. With the widespread emergence of NPS, phenethylamines (PEAs) have become one of the groups abused most which PEAs, along with other stimulants, make up the majority of stimulants. When determining the NPS, the methods for screening and confirmation are crucial which assesses the reliability of testimony. In this study, a set of GC/MS methods employing two derivatizing agents for determining 76 target PEAs in urine was established and further applied for authentic sample analysis. Five PEAs (N,N-DMA, PMMA, 4-CA, amphetamine, and methamphetamine) with contents over their LLOQs were detected in thirteen of the twenty tested samples. In order to compare the result from the GC/MS methods with the previously established LC-MS/MS method, Cohen's kappa coefficient and McNemar's test were applied for statistical analysis. Perfect agreement between GC/MS and LC-MS/MS techniques for determining target PEAs is demonstrated by the Kappa coefficient for each of the five detected targets.