• 분석과학
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• 제6권3호
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• pp.283-288
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• 1993

기체 크로마토그래피를 이용하여 과수 재배용 살균제인 nuarimol의 분석을 위한 최적 조건을 조사하고 사과 중에서의 잔류성을 규명하였다. 사과시료를 methanol로 추출, 여과한 후 4.00% NaCl과 dicholromethane액으로 분리농축하고, alumina 컬럼상에서 1-chlorobutane과 methanol 혼합액으로 정제하여 GLC/ECD로 분석하였다. 0.200와 1.00ppm 표준물 첨가 실험결과 평균 회수율이 79~95%였고, 사과 중 nuarimol의 잔류량은 수확 3일 전 8회 처리시 0.0830ppm이었다. 사과에 대한 안전 사용기간은 수확 7일전 6회 사용이 적당한 것으로 나타났다.

• Journal of Nutrition and Health
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• 제13권4호
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• pp.159-166
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• 1980

Methods for the determination of sterols in sesame oils were studied. The sesame oils were saponified and the sterols isolated from the unsaponifiable matter by Florisil column chromatography, and the individual components were determined by means of gas chromatography. Campesterol, ${\beta}-sitosterol$, stigmasterol were found in sesame oil including unknown Ⅰ and Ⅱ. The use of SE-30 gas chromatographic column allows the slow elution, duplication of peaks and relatively low reproducibility, therefore, 3% OV-17 was suitable for the sterol analysis. The result of this study showed that contents of sterols in sesame oil were campesterol 8.4%, stigmasterol 4.5%, ${\beta}-sitosterol$ 33.9% and others 53.0% involving 8.8% of unknown I and 44.3% of unknown Ⅱ. There has been no specific test available for identifying the sesame oil among common edible oils. But the ratio of sterols in sesame oils allowed the estimation of genuiness. The ratio of sterols vs. campesterol in genuine sesame oils were stigmasterol 0.3- 0.6, ${\beta}-sitosterol$ 3.0-3.8 and unknown Ⅱ 3.0, respectively. The 65 samples were composed of genuine sesame oil 40%, mixed rape seed oil 3%, cotton seed oil 1. 5% others were reused soybean oil or re-extracted oil.

• Applied Biological Chemistry
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• 제35권2호
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• pp.132-138
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• 1992

Methylisothiocyanate에 의한 단백질의 아미노산 배열 결정시 순차적으로 분리되어 나오는 methylthiohydantion 아미노산을 기체 크로마토그라피로 효과적으로 정성 및 정량하기위하여 새로운 silylating reagent인 N-methyl-N-(tert.-butyldimethylsily)trifluoroacetamide를 사용하여 N-tert.-butyldimethylsily MTH 유도체로 silylation 한 후 HP-1 capillary column으로 분석하였다. Cystine을 제외한 21개의 단백질 구성 아미노산을 동정할 수 있었고 지금까지 packed column에서 TMS 유도체로 동정할 수 없었던 arginine도 분리 동정되었다. 2개 이상의 peak를 나타낸 것으로는 hydroxyproline, proline, isoleucine, glycine 및 tyrosine이었고 이중 hydroxyproline은 많은 수의 peak들로 분리되었다. Lysine, histidine 및 arginine은 주입량 $5.0\;nmole{\sim}15.0\;nmole$의 범위에서 나머지는 $2.5\;nmole{\sim}7.5\;nmole$의 범위에서 상관관계를 측정한 결과 고도의 직선 상관관계를 나타내었다(p<0.001). TMS 유도체에 의한 분석은 많은 불순 peak들 때문에 정량분석에 이용할 수 없었다.

• 한국식품과학회지
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• 제28권6호
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• pp.1177-1179
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• 1996

식품포장재에 함유되어있는 톨루엔 및 잔류용제를 용출분석하는 방법으로 headspace gas chromatography (static headspace method)를 이용하였다. 5종(methanol, isopropyl alcohol, ethyl acetate, methyl ethyl ketone, toluene)의 표준용제에 대한 머무름시간과 상대표준편차를 검토해 본 결과, 이상적인 머무름시간의 상대표준편차라 할 수 있는 0.15% 이하로 양호하였으며 재현성도 우수하였다. 인쇄된 포장재를 분석한 결과. 주로 methanol, toluene, methyl ethyl ketone이 검출되었고, methanol은 불검출${\sim}0.939\;mg/m^2$, toluene은 불검출${\sim}1.403{\;}mg/m^2$, methyl ethyl ketone은 불검출${\sim}0.932\;mg/m^2$ 함유 되어있는 것으로 나타났으며, 총 잔류 용제는 불검출${\sim}2.433{\;}mg/m^2$ 함유되어 있는 것으로 나타났다.

• 분석과학
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• 제37권2호
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• pp.123-129
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• 2024

We present a rapid method for the determination of Cs, Sr, and Ba, heat generators found in highly active liquid wastes, by gas-pressurized extraction chromatography (GPEC) using a column containing a cation-exchange resin. GPEC is a microscale column chromatographic technique that uses a constant flow rate of solvent (0.07 mL/min) with pressurized nitrogen gas supplied through a valve. In particular, because this method uses a small sample volume (a few hundred microliters), it produces less chemical waste and allows for faster separation compared to traditional column chromatography. In this study, we evaluated the separation of Cs, Sr, and Ba using GPEC. The eluate from the column (GPEC or conventional column chromatography) was quantitatively analyzed using inductively coupled plasma-mass spectrometry to measure the column recovery and precision. The column reproducibility of the proposed GPEC system (RSDs of recoveries) ranged from 2.7 to 4.1 %, and the column recoveries for the three elements ranged from 72 to 98% when aqueous HCl was used as the eluent. The GPEC results are slightly different in efficiency and separation resolution compared to those of conventional column chromatography because of the differences in the eluent flow rate as well as the internal diameter and length of the column. However, the two methods had similar recoveries for Cs and Sr, and the precision of GPEC was improved by two-fold. Remarkably, the solvent volume required for GPEC analysis was five times lower than that of the conventional method, and the total analysis time was 11 times shorter.

• Journal of Ginseng Research
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• 제13권2호
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• pp.183-188
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• 1989

인삼의 주요 polyacetylens 화합물인 panaxynol, panaxydol 및 panaxytriol의 정량을 위한 GC 분석조건을 확립하였다. 이 때, GC column과 검출기는 SPB-1 fused silica capillary(0.25 mm i, d. $\times$30m, Supelco)와 불꽃이온화검출기(FID)를 사용하였으며 column oven의 온도는 $250^{\circ}C$ 등온이었다. Panaxynol, panaxydol 및 panaxytriol peaks의 retention time은 TMS 유도체화 전의 경우에는 각각 4.2, 5.1 및 6.9분이었으며 TMS유도체화 후에는 각각 4.5, 5.4 및 7.4 분이었다. TMS 유도체화 전의 panaxynol, panaxydol 및 panaxytriol의 정량가능 최소농도는 각각 20, 50 및 100ppm 이었던 데에 비하여, TMS 유도체화 후에는 세 화합물의 정량가능 최소농도가 모두 5ppm의 낮은 수준을 나타내었다. 한편, 홍삼 중의 panaxynol, panaxydol 및 panaxytriol 함량 분석값은 각각 724, 721 과 71$\mu\textrm{g}$/g이었다.

• Archives of Pharmacal Research
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• 제29권4호
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• pp.339-342
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• 2006

A simple high performance liquid chromatographic (HPLC) method was developed for the determination of tolperisone in human plasma. Tolperisone and internal standard (chlorphenesin) were isolated from 1 mL of plasma using 8 mL of dichlormethane. The organic phase was collected and evaporated under nitrogen gas. The residue was then reconstituted with 300 mL aliquot of mobile phase and a 100 mL aliquot was injected onto the $C_{18}$ reverse-phased column. The mobile phase, $45\%$ methanol containing $1\%$ glacial acetic acid and $0.05\%$ 1-hexanesulfonic acid was run at a flow rate of 1 mL/min. The column effluent was monitored using UV detector at 260 nm. The retention times for tolperisone and the internal standard were approximately 7.1 and 8.4 min, respectively. The standard curve was linear with minimal intra-day and inter-day variability. The quantification limit of tolperisone in human plasma was 10 ng/ mL. The proposed method has been applied to the determination of pharmacokinetic profile of tolperisone in Koreans. The T max of tolperisone in Koreans $(0.94{\pm}0.42\;h)$ was not significantly differ from that reported in Europeans (0.5-1 h), but the mean half-life in Koreans $(1.14{\pm}0.27\;h)$ was shorter than that in Europeans $(2.56{\pm}0.2\;h)$. The proposed HPLC method is simple, accurate, reproducible and suitable for pharmacokinetic study of tolperisone.

• 한국환경농학회지
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• 제29권2호
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• pp.165-175
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• 2010

A gas chromatographic (GC) method was developed to determine residues of captan, folpet, captafol, and chlorothalonil, known as broad-spectrum protective fungicides for the official purpose. All the fungicide residues were extracted with acetone containing 3% phosphoric acid from representative samples of five agricultural products which comprised rice, soybean, apple, pepper, and cabbage. The extract was diluted with saline, and dichloromethane partition was followed to recover the fungicides from the aqueous phase. Florisil column chromatography was additionally employed for final cleanup of the extracts. The analytes were then determined by gas chromatography using a DB-1 capillary column with electron capture detection. Reproducibility in quantitation was largely enhanced by minimization of adsorption or thermal degradation of analytes during GLC analysis. Mean recoveries generated from each crop sample fortified at two levels in triplicate ranged from 89.0~113.7%. Relative standard deviations (RSD) were all less than 10%, irrespective sample types and fortification levels. As no interference was found in any samples, limit of quantitation (LOQ) was estimated to be 0.008 mg/kg for the analytes except showing higher sensitivity of 0.002 mg/kg for chlorothalonil. GC/Mass spectrometric method using selected-ion monitoring technique was also provided to confirm the suspected residues. The proposed method was reproducible and sensitive enough to determine the residues of captan, folpet, captafol, and chlorothalonil in agricultural commodities for routine analysis.

• 농약과학회지
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• 제4권2호
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• pp.11-17
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• 2000

분석 대상인 24종 농약을 극성이 다른 캐필러리 칼럼인 DB-17, SPB-608, 및 Ultra-2를 이용하여 전자적압력조절장치(Electronic pressure control, EPC)가 장착된 HP 5890 series II Plus 가스크로마토그래피에서 전자포획검출기로 동시분석법의 최적조건을 모색하였다. 본 실험에서 EPC 시스템의 압력조절기능을 도입하므로써 다음과 같은 분석향상을 얻었다. DB-17, SPB-608, 및 Ultra-2 캐필러리 칼럼에서 EPC 기능없이 동시 분석한 결과 일부 농약들이 분리되지 않았다. 그러나 EPC 시스템의 압력조절 기능을 적용한 결과 vinclozolin과 acetochlor를 제외한 22종 농약 모두 SPB-608 캐필러리 칼럼에서 동시 분석되었다. 또한 농약들의 분리 시간에도 영향을 주어 총 분석시간이 단축되었다. 즉 EPC 시스템 없이 분석한 시간이 $61{\sim}81$분인데 반해 EPC 시스템도입으로 45분으로 단축되었다. 각 농약들에 대한 검출한계는 $0.1{\sim}12.9$ ng/mL 검출되었다.

• 분석과학
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• 제13권4호
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• pp.484-493
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• 2000

생물시료 중 존재하는 알킬페놀류, 클로로페놀류 및 비스페놀 A의 동시분석을 기체크로마토그래피-질량분석기-선택이온검색법에 의해 수행하였다. 시료 중 페놀류는 유기용매로 추출하고 정제과정은 Florisil과 silica 컬럼을 비교분석하였다. 회수율 실험은 각 생물시료에 1-ppm 정도를 첨가하여 수행하였다. 이들의 회수율은 83-116% 정도로 나타났고, 표준편차는 약 2.4-11.9%로 나타났다. 페놀류의 검출한계를 증진시키기 위하여, trimeaylsilyl(TMS) 유도체 방법을 도입하였다. 유도체화 시키지 않은 페놀과 TMS 유도체화된 페놀류의 기체크로마토그래피 성질을 연구하였다.