SYNTHESIS OF 2-THIOTHIAZOLIDINE-4-CARBOXYLIC ACID AND ITS CHROMATOGRAPHY IN RAT AND HUMAN URINE

2-Thiothiazolidine-4-carboxylic acid (TTCA), the urinary biological mo nitoring marker for carbon disulfide in humans was synthesized by reac ting carbon disulfide with L-cystine. Validation of TTCA purity requir ed elemental as well as mass spectral and chromatographic analyses. Tw o reversed-phase high-performance liquid chromatographic columns in se ries were necessary to resolve picomole amounts of TTCA from rat and h uman urine background peaks on detection at 272 nm even after prior di ethyl ether extraction from acidified urines in the presence of satura ted 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 ra nge (0.0165-4.95 nmol injected mass) with a coefficient of variation o f 8.6%. The detection limit was about 100 nM (1.5 pmol injected mass).