Quantitative determination of ursodeoxycholic acid and its deuterated derivative in human bile by gas chromatography-mass fragmentography.

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Abstract
Deuterium-labeled ursodeoxycholic acid (UDCA-d2) was synthesized from cholic acid by heterogeneous catalytic reduction of the 11,12-unsaturated bile acid with D2 gas. A new method for the simultaneous determination of UDCA, UDCA-d2, related bile acids and cholesterol in human bile was developed by gas chromatography-mass fragmentography of the methyl ester trimethylsilyl ether derivatives. The glycine conjugate of 5.beta.-chol-3-en-24-oic acid was prepared from lithocholic acid and used as an internal standard. Calibration plots gave a good linear relationship over the range of 100-500 ng of each compound. Their recoveries (95-99%) relative to the internal standard suggested that the present method is sufficiently accurate for the practical analysis of these bile acids in human bile. The method was applied to investigate the fate of UDCA-d2 orally administered to a patient with complete bile fistula.