• Bulletin of the Korean Chemical Society
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• 제33권5호
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• pp.1693-1698
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• 2012

A headspace gas chromatographic mass spectrometric (GC-MS) assay method was developed for the simultaneous determination of methyl tertiary butyl ether (MTBE), $tert$-butyl alcohol (TBA) and benzene, toluene, ethyl benzene and xylene (BTEX) in soil contaminated with gasoline. 2 g of soil sample were placed in a 10 mL headspace vial filled with 5 mL of phosphoric acid solution (pH 3) saturated with NaCl, and the solution was spiked with fluorobenzene as an internal standard and sealed with a cap. The vial was heated in a heating block for 40 min at $80^{\circ}C$. The detection limits of the assay were 0.08-0.12 ${\mu}g$/kg for the analytes. For five independent determinations at 10 and 50 ${\mu}g$/kg, the relative standard deviations were less than 10%. The method was used to analyze fifty six soil samples collected from various regions contaminated with gasoline in Korea. The developed method may be valuable for the monitoring of the analytes in soil.

• Bulletin of the Korean Chemical Society
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• 제25권6호
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• pp.806-808
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• 2004

A gas chromatography/mass spectrometric assay method has been developed for the simultaneous determination of icing inhibitors, ethylene glycol monomethyl ether and diethylene glycol monomethyl ether in ground water contaminated with JP-8. Ethylene glycol monobutyl ether and ethylene glycol monoethyl ether were used as the internal standard and surrogate, respectively. 100 mL of ground water was extracted twice with 20 mL of methylene chloride. The extract was concentrated to dryness, dissolved with 100 ${\mu}$L of methanol and analyzed by GC-MS (SIM). The use of an Innowax column gave the peaks good chromatographic properties, and the extraction of these compounds from samples gave recoveries of about 50% with small variations. The method detection limits of the target compounds were in a range of 0.5-0.8 ng/mL in ground water.

• 분석과학
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• 제15권5호
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• pp.445-450
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• 2002

해수에 함유되어 있는 요오드화합물의 총량을 휘발성 유기물로 유도체화 후 측정하는 방법을 확립하였다. 이 방법은 요오드 음이온은 요오드로 산화시킨 후 2,6-dimethylphenol과 반응하여 4-iodo-2,6-dimethylphenol로 전환시켜 ethylether로 1단계 추출 후 gas chromatography-mass spectrometry (selected ion monitoring)로 측정하는 것으로 구성되어 있다. Iodate는 ascorbic acid 와 acetic acid로 요오드 음이온으로 환원시킨 후 요오드 음이온 측정법과 동일하게 수행하였다. 이 방법은 검출한계가 해수에서 0.1 ng/ml이었으며 검량선은 0.9997의 좋은 상관계수값을 보였다. 이 방법은 또한 재현성이 우수하고 간단하여 해수에 인체의 필수원소인 요오드를 낮은 농도까지 분석하는데 유용하게 사용될 수 있다고 사료된다.

• Environmental Analysis Health and Toxicology
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• 제16권4호
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• pp.181-188
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• 2001

A gas chromatographic method was established for the simultaneous determination of urinary nicotine and cotinine. The analytes in basified urine containing a sufficient amount of Na$_2$S0$_4$were extracted into dichloromethane by vigorous shaking. Into the transferred organic phase was added a small amount of acidified methanol (0.5 N HCI in methanol), followed by concentrating the mixture to dryness using a mild stream of nitrogen gas. The concentrate was reconstituted with methanol and the final solution analyzed using the gas chromatograph equipped with the nitrogen-phosphorus detector. The reproducibility tests showed coefficients of variation less than 11％ for both compounds. The percent recovery for both analytes ranged from 88 to 103％. The estimated method detection limits for nicotine and cotinine were 0.60 and 5.1 ng/mL, respectively. Extraction efficiencies for both nicotine and cotinine apparently declined without the addition of Na$_2$S0$_4$into the urine. Moreover, the absence of methanolic HCI in the extract resulted in almost complete evaporation of nicotine and partial loss of cotinine during the concentration process, indicating that the formation of nicotine-HCI and cotinine-HCI species is prerequisite to the suppression of the loss of both compounds.

• 한국환경과학회지
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• 제18권12호
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• pp.1369-1381
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• 2009

The simultaneous determination of residual pesticides was developed using a gas chromatography. In this study, a simple and reliable methodology was improved to detect 175 kinds of residual pesticides by a liquid-liquid extraction procedure, followed by chromatographic analysis by gas chromatography. The 175 kinds of residual pesticides was classified into 4 groups according to the chemical structure, column type, resolution and sensitivity. The soybean sample selected for recovery experiment was not detected any pesticides. The recovery rates were ranged from 70.6% to 119.7% in most pesticides. The relative standard deviation (RSD 0.3~5.6%) was lower than 5.6% in all cases. The limits of detection (LOD) was lower than the maximum residue levels established by Korean legislations. The method has been successfully applied to the analysis of approximately 130 real samples.

• 한국식품위생안전성학회지
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• 제18권2호
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• pp.43-50
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• 2003

A liquid chromatographic method, using matrix solid-phase dispersion (MSPD) is developed for the extraction of residual furazolidone in chicken eggs. Blank or fortified egg samples (0.5 g) were blended with Octadecylsilyl (Bulk $C_{18}$, 40${\mu}{\textrm}{m}$, 18%. load, endcapped. 2 g) derivatized silica. After homogenization, $C_{18}$/egg and Na$_2$S $O_4$matrix were transferred to a column made of 10 ml glass syringe and filter paper and compressed 4.0∼4.5 ml volume. The column was washed with 8 ml of hexane and dried under $N_2$ gas. Furazolidone was eluted with acetonitrile (8 ml) under gravity. The eluate containing furazolidone was free from interfering compounds when analyzed by HPLC with UV detection (365 nm, photodiode array). Calibration curves were linear (r = 0.99985) and inter- (1.47%) and intra-assay (5.29%) variabilities for the concentration range examined (7.8∼497 ng/g of eggs, 20 ${mu}ell$ injection volume) were indicative of an acceptable methodology for the analysis of furazolidone. Average recovery of furazolidone added to egg was 96.2%. The limit of detection for the proposed method was 1 ng/g for furazolidone. The method using MSPD is proposed as an alternative assay to the classical method which involves the use of large volumes of a harmful solvent and requires a long tedious separation and clean-up processes prior to its determination.

• 한국환경농학회지
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• 제23권4호
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• pp.245-250
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• 2004

An analytical method was developed to determine monocrotophos residues in apple, citrus, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Monocrotophos was extracted with acetone from apple, citrus and moist soil samples. The extract was concentrated, added with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives. Dichloromethane partition was then followed to recover monocrotophos from the aqueous phase. Silica gel column chromatography was employed to further purify the extract prior to HPLC determination. Reverse-phase HPLC using an oct-adecylsilyl column was successfully applied to separate and quantitate the monocrotophos residue in sample extracts at the wavelength of 230 nm. Overall recoveries of monocrotophos from fortified samples averaged $95.3{\pm}2.1%$ (n=6), $970{\pm}0.7%$ (n=6), and $92.8{\pm}4.3%$ (n=12) for apple, citrus, and soil, respectively. The proposed method was quite reproducible and sensitive enough to replace the troublesome gas-liquid chromatographic analysis for monocrotophos residues.

• 약학회지
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• 제37권1호
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• pp.54-65
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• 1993

A method for the determination of 16 residual pesticides in crude deugs was examined. Crude drug was extracted with acetonitrile/water solution and the extract was partitioned between hexane/CH$_{2}$Cl$_{2}$ and NaCl saturated water. The organic layer was passed through cleanup column and subjected to the GC/ECD or GC/NPD analysis. Essential oil components in crude drug interfere with the analysis, and sulfuric acid treatment was adapted to overcome this interference.

• KSBB Journal
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• 제18권1호
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• pp.74-77
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• 2003

대표적인 부패산물들로 잘 알려진 indole, skatole, 그리고 $\rho$-cresol 등을 측정하기 위한 방법으로 HPLC, spectrophotometric 법, 그리고 GC 및 GC/MSD 방법 등이 있으며, 수십년 간에 걸쳐 이러한 물질들의 분석이 이루어져 왔다. 본 연구에서는 많은 전처리 과정을 생략하여 분석물의 손실을 최소화하면서 GC 및 GC/MSD를 이용하여 쉽고 빠르게 측정할 수 있는 조건과 방법을 확립하였다. 측정사료는 건강한 성인 남녀의 분변이었으며, 내부 표준물질로 4-isopropylphenol을 사용하였으며, 분변 중 indole의 함량은 10~90 ppm 수준이었으며, skatole의 경우에는 약 40 ppm 정도로 검출되었다. 또한, $\rho$-cresol은 30~300 ppm 수준으로 그 분포 범위가 아주 넓게 나타났었다. GC/MSD를 이용하여 시료 중상기 물질들을 정성적으로 정확히 확인할 수 있었다. DB-17 capillary 컬럼을 이용하여 시료의 전처리 과정을 생략하여도 분석하려던 부패산물의 정성 및 정량에 방해되는 불순 peak는 없었고, 분리능도 매우 우수하였으므로 보다 빠르고 신속하게 상기 물질들을 확인할 수 있었다. 향후 본 연구를 통해 개발된 신속분석법이 분변에 존재하는 주요 부패산물들의 정량에 유용하게 사용되리라 판단된다.

• 한국식품과학회지
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• 제8권2호
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• pp.85-89
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• 1976

Gas chromatography를 이용하여 methylglyoxal, diacetyl 및 triose reductone과 같은 dicarbonyl류(類)를 분리측정(分離測定)할 수 있는 조건(條件)을 실험(實驗)하였던 바 다음과 같은 결과(結果)를 얻었다. 1. MG, DAc, DTR의 혼합물(混合物)에 OPD를 반응시켜 quinoxaline 유도체(誘導體)를 만들고 이것을 클로로포름으로 추출(抽出)하면 MG 및 DAc는 거의 100%추출(抽出)되었고, DTR은 에틸에테르에 추출(抽出)되었다. 2. SE-30을 충진제로하여 얻어진 column 조건(條件)에서 MG-OPD와 DAc-OPD는 완전히 분리측정(分離測定)할 수 있었다. 3. 당류중(糖類中) glucose의 OPD 축합물형성조건(縮合物形成條件)은 D-glucose 180mg을 0.1N-NaOH 용액 10ml에서 5분간(分間) 가열후 OPD와 반응(反應)시켜 pH 6. 0에서 클로로포름으로 추출(抽出)하여 GLC에 겉면 5개의 peak가 나타났고, 그 중에서 2개는MG-OPD와 DAo-OPD임을 확인하였다. 그러나 중성(中性) 및 산성가열(酸性加熱)인 경우는 peak가 확실치 않았다.