Synthesis of 2-thiothiazolidine-4-carboxylic acid and its chromatography in rat and human urine

被引:9
作者
Cox, C [1 ]
Hee, SSQ [1 ]
机构
[1] UNIV CINCINNATI,MED CTR,DEPT ENVIRONM HLTH,CINCINNATI,OH 45267
来源
JOURNAL OF CHROMATOGRAPHY B-BIOMEDICAL APPLICATIONS | 1996年 / 679卷 / 1-2期
关键词
2-thiothiazolidine-4-carboxylic acid; carbon disulfide;
D O I
10.1016/0378-4347(96)00033-3
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
2-Thiothiazolidine-4-carboxylic acid (TTCA), the urinary biological monitoring marker for carbon disulfide in humans was synthesized by reacting carbon disulfide with L-cystine. Validation of TTCA purity required elemental as well as mass spectral and chromatographic analyses. Two reversed-phase high-performance liquid chromatographic columns in series were necessary to resolve picomole amounts of TTCA from rat and human urine background peaks on detection at 272 nm even after prior diethyl ether extraction from acidified urines in the presence of saturated sodium chloride. The isolation procedure for TTCA from urine had a recovery of 94.0 +/- 8.1% in the linear 1.1-330 mu M concentration range (0.0165-4.95 nmol injected mass) with a coefficient of variation of 8.6%. The detection limit was about 100 nM (1.5 pmol injected mass).
引用
收藏
页码:85 / 90
页数:6
相关论文
共 17 条
[1]  
*AM C GOV IND HYG, 1991, DOC BIOL EXP IND
[2]  
[Anonymous], BIOL MONITORING INTR
[3]  
*ASTM, 1989, 1989 ANN BOOK ASTM S, P45
[4]   EVALUATION OF OCCUPATIONAL EXPOSURE TO CARBON-DISULFIDE BY BLOOD, EXHALED AIR, AND URINE ANALYSIS [J].
CAMPBELL, L ;
JONES, AH ;
WILSON, HK .
AMERICAN JOURNAL OF INDUSTRIAL MEDICINE, 1985, 8 (02) :143-153
[5]  
COX C, 1996, UNPUB TOXICOL IND HL
[6]  
COX C, UNPUB AM J IND MED
[7]  
DEBAUN JR, 1974, XENOBIOTICA, V4, P101, DOI 10.3109/00498257409049350
[8]   SIMULTANEOUS MULTIELEMENTAL ANALYSIS OF SOME ENVIRONMENTAL AND BIOLOGICAL SAMPLES BY INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION-SPECTROMETRY [J].
HEE, SSQ ;
BOYLE, JR .
ANALYTICAL CHEMISTRY, 1988, 60 (10) :1033-1042
[9]  
KIVISTO H, 1995, ARCH TOXICOL, V69, P195
[10]  
KOPECKY J, 1984, B SOC CHIM BELG, V93, P231