• 한국식품영양과학회지
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• 제32권3호
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• pp.320-324
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• 2003

단백질 구성 아미노산 분석을 위한 효과적인 가수분해 방법을 찾기 위하여 0.3% tryptamine을 함유한 6M formic acid와 6M HCI을 표준 아미노산과 단백질 표준품인 bovine serumn albumin 가수분해에 적용하여 표준아미노산의 회수율과 bovine serum albumin의 아미노산 조성을 분석하였고 GC에 의한 효과적인 아미노산 분석을 위하여 새로운 유도체인 butylthiocarbamyl-trimethylsilyl(BTC-TMS)유도체를 개발하여 분석한 결과는 다음과 같았다 표준아미노산의 회수율은 6M formic acid에 의한 가수분해방법이 6M HCI에 의한 가수분해 방법보다 상당히 정확하였고 특히 산 가수분해에서 tryptamine의 존재하에서도 잘 파괴되는 tryptophan의 경우 formic acid가수분해가 HCI가수분해보다 1.5배정도 높은 회수율을 보였다. Bovine serum albumin의 아미노산 조성을 583 아미노산 잔기로 환산하여 나타내었을 경우도 formic acid에 의한 가수분해가 HCI가수분해 경우보다 훨씬 정확하였고 이 때 tryptophan의 회수율도 훨씬 높게 나타났다. 다만 서열분석에서 분석되지 않는 cystine이 formic acid 가수분해시 분석되고 있어 이에 대한 정확한 검정이 필요하였다. BTC-TMS 유도체는 GC분석시 극성이 다소 낮은 DB-l7 column으로 분리가 잘되었고 재현성도 좋았으나 GC분석을 위한 대부분의 유도체에서와 마찬가지로 몇 가지 아미노산에서 두 개의 peak로 나타나는 결점이 있었다.

• 한국연초학회지
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• 제15권2호
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• pp.174-184
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• 1993

This is to investigate the methodology for the simultaneous determination of Wk, mk and TSNA using gas chromatography(GC) in combination with chemiluminescence detector, thermal energy analyzer(TEA) . The simultaneous analysis has been estimated by evaluating tobacco. The TEA was linked to GC equipped with non -polar SPB -5 fused silica capillary column which was introduced into the ceramic pyrolysis tube by the point of 16cm from the end of TEA. Quantification was carried out by internal standardization with WDPA after calibration of retention times and response factors with authentic nitrosoamines. It was demonstrated that WDPA was most preferable as internal standard for the simultaneous analysis. The recoveries of the internal standard were in the range of 83∼96% . Nitrosoamines in this method were detected with determination limit of 0.1ng and was made by a straight line in calibration curve by TEA response. The suitability of nitrosoamines extraction in tobacco leaf was investigated. It was most suitable to extract nitrosoamines from tobacco leaves with 0.01 M NaOH within a period of 8 hours. Thimerosal as an antibacterial agent was added to NaOH solution to prevent artifactual formation. The fractionation and the purification of nitrosoamines form alkaline extracts were conveniently performed using Extrelut multilayer column and dichloromethane. Reproducible and reliable results were obtained for the determination of nitrosamines in a relatively short time compared to previous known method. TSNA contents in burley were about 4 times higher as those in the fluecured tobacco.

• 한국식품과학회지
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• 제24권2호
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• pp.171-176
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• 1992

더덕(Codonopsis lanceolata)의 휘발성 향기성분을 분석하기 위해 gas co-distillation(GCD), solvent extraction/fractionation(SLF), headspace sampling(HSS) 방법을 사용하여 향기성분을 분리농축하고 분석 비교한 결과 SEF와 HSS 방법으로 얻은 농축물들의 향이 원래의 더덕향과 가장 유사했으며 gas chromatogram들의 양상도 비슷했으나 peak들의 크기에 있어서 차이를 보였다. SEF 농축물에서는 달콤한 향을 기리고 HSS 농축물에서는 풋내를 비교적 강하게 느낄 수 있었으나 GCD 농축물의 경우 일정 증류시간이 지나면 한악취를 느낄 수 있었다. SEF와 HSS 방법은 GCD에 비해서 적은 조작 단계로 손쉽게 빠른 시간내에 분리 농축이 가능했다. 농축한 향기성분은 GC-MS와 극성이 다른 두 column을 사용한 GC-RI system을 이용하여 확인하였다. 특히 GC-RI는 isomer의 확인에 효과적이었으며 극성 FFAP column은 극성 화합물의 확인에 보다 적합했다. 35가지의 향기성분들을 동정하였는데 그중 24개의 성분들은 simultaneous distillation extraction 농축물에서는$^{(5)}$ 확인되지 않았던 향기성분들이다. 화인된 성분들중 trans-2-hexenal, cis-3-hexen-1-ol, trans-2-hexen-1-ol, hexanol은 더덕의 풋내를, 1-octen-3-ol은 신선한 풍미를 그리고 amyl propionate를 비롯한 다수의 에스터 화합물 등은 더덕 특유의 달콤한 향에 복합적으로 작용할 것으로 추정된다.

• 한국식품영양과학회지
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• 제28권5호
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• pp.980-983
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• 1999

The contents of sterols and stanols in vegetable oils and mist oil were analyzed by gas chromatography using a capillary column. The total sterol contents showed high values of 0.67~0.89g/100g in corn oil, rice bran oil, red pepper seed oil and sesame oil. Mist oil, a byproduct of soybean oil manufacture, was a suitable raw material for the production of stanol since it showed high sterol content (10.2g/100g). In the hydrogenation of sterol contained in mist oil using Pd catalyst, the effects saponification of oil were examined. The conversion of sterol to stanol was improved by a factor of 4~5 through saponification of oil, compared to the reaction without saponification.

• 한국지하수토양환경학회:학술대회논문집
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• 한국지하수토양환경학회 2005년도 총회 및 춘계학술발표회
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• pp.195-198
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• 2005

A solid-phase microextraction and gas chromatography-mass spectrometry for the extraction and analysis of methyl-tert-butyl ether has been described. methyl-tert-butyl ether was extracted from aqueous solution using SPME fiber coated polydimethylsiloxane and analysed by GC-MS with capillary column. Extraction parameters and chromatographic separation conditions were optimized. The applied method represented good analytical performance in terms of precision (3-8%, RSD) and accuracy(93-102%, mean recovery) with a method detection limit of 0.03 ppb.

• 한국연초학회지
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• 제23권2호
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• pp.162-167
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• 2001

This study was carried out to quantitatively determine phenol compounds in smoke total particulate matter(TPM) to evaluate the qualititive characteristics of flue-cured tobacco varieties(NC82, KFl14 and KFl18). After collecting The TPM by using smoking machine, the concentration of phenol compounds were analyzed by gas chromatography as their trimethylsilyl derivative on a fused capillary column bonded with a 5％ PE ME siloxane stationary phase. In all the flue-cured tobacco varieties, the major phenol components were monohydroxy compounds. The order of the highest concentration of total phenol compounds in TPM was NC82, KF114 and KFl18 but the contents of dihydroxy compound in the KFl18 was higher than those of NC82 and KF114.

• 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.

• 대한화학회지
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• 제30권4호
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• pp.369-376
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• 1986

모세관 기체-액체프로마토그래피(GLC)에 의해 인도네시아산 Costus speciosus중의 diosgenin을 정량하기 위해 가수분해 및 추출, 아세틸화 반응 및 GLC의 측정 조건등을 검토하였다. 건조된 diosgenin분말 1.20g을 3N HCI과 xylene의 혼합용액으로 95∼100${\circ}C$에서 4시간 환류시킨 다음 xylene층을 분리하였다. Xylene을 증발시켜 날려보내고 20:80의 acetic anhydride-pyridine을 가하고 30분간 환류시켜 아세틸화시킨 후 diethyl ether로 추출하였다. 무수 $Na_2SO_4$로 탈수시키고 ether를 날려 보낸 다음 찌끼를 n-hexane 5.00ml에 녹여 GLC로 분석하였다. SE-30 25m ${\times}$ 0. 33mm의 모세관을 사용하였고 컬럼온도는 180${\circ}$에서 270${\circ}C$까지 10${\circ}C$/min의 속도로 온도를 상승시켰다. 운반기체 $N_2$의 유속은 2ml/min이었고 FID로 검출하였다. Diosgenin의 분석결과는 0.281%이었고, 상대표준편차는 1.8%로서 재현성이 좋았다.

• 대한화학회지
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• 제35권5호
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• pp.560-568
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• 1991

국내에서 현재 규제되고 있는 농약에 대해 신속, 간단한 동시분석법이 연구되었다. 시료는 아세톤과 메탄올로 추출하고 물을 가한 다음, $CH_2Cl_2$로 분배시킨다. 추출물은 Bio-Beads S-X3 컬럼에서 cyclohexane-methylene chloride의 용출액 11ml를 받아 불순물을 분리, 제거하고 ECD/NPD가 병렬되게 BP-1(methyl silicone) 모세관 컬럼에 연결된 기체 크로마토그래피로 분석한다. 농약 첨가에 의한 평균 회수율은 쌀에서 83% 이상이었고, 콩에서 3종 농약을 제외하면 81% 이상이었다. 검출한계는 쌀에서 0.002 ppm(${\alpha}$-BHC 등)~0.3 ppm(carbaryl 등) 이었다.

• 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.