• 한국산업보건학회지
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• 제10권1호
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• pp.208-222
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• 2000

This study was conducted to supplement limit of previous study, The objectives of this study were to select optimal conditions of high performance liquid chromatography(HPLC) operation for detecting urinary 2-thiothiazolicline-4-carboxylic acid(TTCA) and thiocarbamide simultaneously, and to evaluate recovery rates for various liquid-liquid extration method of these metabolites, The results are as follows : 1. The urinary TTCA and thiocarbamide were separate sharply when flow rate is $0.7m{\ell}/min$, using a series $C_8$ and $C_{18}$ column, 50 mM $KH_2PO_4$ : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase. The retention time was TTCA, $12.07{\pm}0.11$(mean${\pm}$SD, n=06), thiocarbamide, $7.85{\pm}0.01$ (mean${\pm}$SD, n=6), respectively. The calibration curve for TTCA and thiocarbamide was linear within the range 0.05 to $30{\mu}g/m{\ell}$. 2. By the liquid-liquid extration, butanol extration with $(NH_4)_2$ as a salting-out reagent was used as a simultaneous extration method for these metabolites in acid state, and recovery rates of this method are urinary TTCA, $49.6{\pm}17.7$ (mean${\pm}$SD, n=16), thiocarbamide, $43,9{\pm}5.50$ (mean${\pm}$SD, n=16), respectively 3. The precision(pooled coefficients of variation for 4 concentration) of the urinary thiocarbamide analysis was 0.03754 by butanol liquid-liquid extraction with $(NH_4)_2$ as a salting-out reagent, and TTCA was 0.04082 by ethyl acetate liquid-liquid extration with $(NH_4)_2$ as a salting out reagent The above results show that the butanol liquid-liquid extraction with $(NH_4)_2$ as a salting-out reagent in acid state, and using a series $C_8$ and $C_{18}$ column, 50 mM $KH_2PO_4$ : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase are suitable for the analysis of urinary TTCA and thiocarbamide simultaneously. The detection limit of TTCA and thiocarbamide was about $0.17{\mu}g/m{\ell}$, $0.07{\mu}g/m{\ell}$.

• 한국산업보건학회지
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• 제6권2호
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• pp.202-208
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• 1996

The purposes of this study are the identification and determination of metabolites in the isolated rat liver perfusate of carbon disulfide by two-dimentional thin-layer chromatography and high performance liquid chromatography for understanding the metabolism of carbon disulfide. 2-Thio-thiazolidine-4-carboxylic acid(TTCA) was synthesized by the reaction of carbon disulfide and cysteine, and confirmed by two-dimentional thin-layer chromatography, high performance liquid chromatography, UV spectroscopy, and IR spectroscopy. The absorbance of UV detector for the simultaneous determination of TTCA and thiocarbamide was 254 nm although their maximum spectra were 273 nm and 237 nm, respectively. Two kinds of the developing solvent in the two-dimentional thin-layer chromatography were 2-butanol : 80% HCOOH : $H_2O$ (7 : 2 : 1) as the first developing solvent and 2-propanol : $H_2O$ (4 : 1) as the second developing solvent. After perfusion of carbon disulfide ($8274.23{\mu}mol$), the amount of TTCA and thiocabamide of the perfusate(100 ul) were $12.02-16.4{\mu}mol$ and $5.25-8.15{\mu}g$, respectively. The mean amount of them were $14.08{\mu}mol$ and $6.41{\mu}mol$ respectively, and the former was 2.20 times greater than the latter. For conforming the mechanism of formations of TTCA and thiocarbamide in vivo, we have to clarify whether the reactions between carbon disulfide and ammonia, ammonium salts, amides, cysteine, cystine, or proteins will be formed in vitro.

• Bulletin of the Korean Chemical Society
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• 제30권7호
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• pp.1667-1670
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• 2009

• Environmental Analysis Health and Toxicology
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• 제16권2호
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• pp.97-102
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• 2001

FMOs (Flavin-containing monooxygenases, EC1.14.13.8)는 다양한 종류의 식품, 약물이나 기타 외래 유래물질 (xenobiotics)를 산화시키는 NADPH와 $O_2$ 의존성 약물대사효소이다. 현재까지 5종의 subfamily가 존재하는 것으로 보고되어 있으며 그 중 잘 알려진 FMO3는 대표적 인 subfamily로서 주로 간에 존재한다 사람FMO에 관한 연구는 최근 들어 활성화되기 시작했으며 질소, 황이나 인 등을 포함하는 친핵성 (nucleophilic) 화합물이 대표적인 기질로 보고되어 있다. 본 연구에서는 thiocarbamide를 포함하고 있는 화합물에 대한 사람의 FMO3의 기질 특이성을 알아보고자 하였다. 사람 FMO3를 baculovirus system을 이용하여 대량으로 발현시킨 후 그 microsomal FMO3를 분리하여 thiocholine assay를 시행하였다. 그 결과 methimazole, thiourea, and phenylthiourea는 낮은 $K_{m}$ (4-10$\mu$M)간을 갖는 반면, 이보다 기질의 크기가 큰 1 ,3-diphenylthiourea, 1, 3-bis (3, 4-dichlorophenyl)-2-thiourea, 1, 1-dibenzyl-3-phenol-2-thiourea에서는 효소활성이 나타나지 않았다. 이는 사람 fM01과 비교하여 볼 때 큰 차이는 없었으며, 다른 pig, guinea pig, rat, rabbit에서 보다 받아들일 수 있는 기질의 크기가 더 제한적임을 알 수 있었다.

• Bulletin of the Korean Chemical Society
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• 제25권7호
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• pp.1019-1024
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• 2004

The present paper is focused on simultaneous sorption concentration of gold (III) and silver (I) from thiocyanate solutions using high-selective anion exchanger AN-25 and subsequent separation of these ions at various concentrations of thiocarbamide (eluent). As a result, silver (I) ions are completely eluted from AN-25 and gold (III) ions remain in the resin phase and can be determined directly in the solid phase by diffuse reflection spectroscopy. It is proposed to use the sorption-spectroscopic method for Au(III) determination in aqueous solutions. The calibration curve is linear in the concentration range of 1-19 mg/L (sample volume is 10.0 mL) and the detection limit is 0.05 ${\mu}g/mL$. The presence of Cu(II), Co(II), Fe(II) do not hinder this determination. Au(III) was determined in industrial solutions.