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부타놀 추출법을 이용한 2-thiothiazolidine-4-carboxilic acid와 thiocarbamide의 동시정량에 관한연구

Other Titles
Simultaneous analysis for 2-thiothiazolidine-4-carboxilic acid and thiocarbamide using butanol extraction method
Authors
이상회  ;  송재석  ;  윤영식  ;  김치년  ;  원종욱  ;  노재훈
Citation
Journal of Korean Society of Occupational and Environmental Hygiene (한국산업위생학회지), Vol.10(1) : 208-222, 2000
Journal Title
Journal of Korean Society of Occupational and Environmental Hygiene (한국산업위생학회지)
ISSN
1226-4326
Issue Date
2000
Keywords
2-thiothiazolidine-4-carboxylic acid ; Thiocarbamide ; high performance liquid chromatography ; liquid-liquid extration
Abstract
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 C18 column, 50 mM KH2PO4 : acetonitrile (93.5 : 6.5) and pH 3.5 as a mobile phase. The retention time was TTCA, $12.07{\pm}0.11$(mean±SD, n=06), thiocarbamide, $7.85{\pm}0.01$ (mean±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±SD, n=16), thiocarbamide, $43,9{\pm}5.50$ (mean±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 C18 column, 50 mM KH2PO4 : 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 $0.17{\mu}g/m{\ell}$, $0.07{\mu}g/m{\ell}$.
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