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目的:建立一种高灵敏的熊胆粉中牛磺熊去氧胆酸含量的测定方法。方法:以吡啶-苯甲酰氯为柱前衍生化试剂,以RP-HPLC(UV)测定牛磺熊去氧胆酸衍生产物的含量。结果:冰浴下衍生化反应,密封,室温存放24h。色谱条件C18色谱柱,检测波长235nm;流动相:甲醇-水-四氢呋喃(90∶6∶4)为流动相;线性范围:2.8×10-6～3.6×10-6mg/L,最低检测限14ng,用于熊胆粉实际样品的分析,结果满意。结论:方法灵敏、准确,为熊胆粉中牛磺熊去氧胆酸的分析提供了一种方法。
Objective: To establish a highly sensitive method for the determination of tauroursodeoxycholic acid in bear bile powder. Methods: The pyridine-benzoyl chloride was used as pre-column derivatization reagent to determine the content of tauroursodeoxycholic acid derivative by RP-HPLC (UV). Results: Derivatization under ice bath, sealed and stored at room temperature for 24h. The mobile phase consisted of methanol-water-tetrahydrofuran (90: 6: 4) as mobile phase. The linear range was 2.8 × 10-6 ~ 3.6 × 10-6mg / L with the detection limit of 14ng , For the analysis of the actual samples of bear gall powder, the results are satisfactory. Conclusion: The method is sensitive and accurate, and provides a method for the analysis of tauroursodeoxycholic acid in bear bile powder.