Research on Change of Constituents of Bear Bile Powder During Production Process of Tanreqing Capsules by HPLC-MS/MS / 中国药学杂志

ABSTRACT

OBJECTIVE: To identify the chemical components of bile acids from bear bile powder, the intermediate of bear bile powder and Tanreqing capsules by HPLC-MS/MS. METHODS: All samples were extracted with 70% methanol(V/V), and an Ultimate XB C18 column (4.6 mm×250 mm, 5 μm) was employed for separation with acetonitrile-0.1% formic acid as mobile phase in gradient elution. The MS spectrum was acquired in both positive and negative ion mode using ESI ion source. The chemical components were identified by the second mass spectrometric pyrolysis fragments, chromatographic peak retention time and fragmentation regularity summarized from the reference standards and the available literature. RESULTS: A total of 33 compounds were successfully identified or tentatively predicted, and six chemical compounds including tauroursodeoxycholic acid, taurochenodeoxycholic acid, ursodeoxycholic acid, chenodeoxycholic acid, 7α-hydroxy-3-oxo-5β-cholanic acid and one unknown constituent were finally transferred to Tanreqing capsules through the intermediate of bear bile powder. Moreover, 21 new chemical compounds (major ingredients of free bile acids) were generated during the production process of the intermediate, and 19 components were also detected in Tanreqing capsules. CONCLUSION: The investigation of the change of constituents in bear bile powder during Tanreqing capsules production provides a basis for the quality control and evaluation of Tanreqing capsules during production process.