【摘要】 目的建立柱前衍生HPLC-UV法测定人工牛黄中猪去氧胆酸含量的方法。方法以2-萘基溴甲基酮为衍生试剂、三乙胺为催化剂、60℃水浴条件下对猪去氧胆酸进行衍生,采用HPLC-UV法测定人工牛黄中猪去氧胆酸含量。结果当衍生试剂与猪去氧胆酸的摩尔比>20∶1,催化剂与猪去氧胆酸的摩尔比>15∶1,在60℃水浴条件下反应50 min时,衍生反应完全。猪去氧胆酸在0.1~2μg范围内线性关系良好(r=0.999 7),平均回收率为97.85%(RSD=1.6%)。人工牛黄样品中猪去氧胆酸的含量为4.12%。结论本方法灵敏度高、准确可靠、稳定性和重复性好,可用于测定人工牛黄中猪去氧胆酸的含量。更多还原

【Abstract】 Objective To establish a pre-column derivation HPLC-UV method for the content determination of hyodeoxycholic acid in artificial calculus bovis. Methods The hyodeoxycholic acid was derived by 2-bromo-2’-acetonaphthoneat using triethylamine as the catalyst in 60 ℃ water bath. After that, a HPLC-UV method was established to determine the content of hyodeoxycholic acid in artificial calculus bovis. Results When the derivatising time at 60 ℃ water bath was 50 min, the radio of the molar amount of derived reagents and hyodeoxycholic was over 20:1 and the radio of catalyst and hyodeoxycholic was over 15:1; the reaction was completed. The calibration curve was linear within the range of 0.1–2 μg for hyodeoxycholic acid(r=0.999 7), and the average recovery was 97.85%(RSD=1.6%). In this sample, the content of hyodeoxycholic is 4.12%. Conclusion The method is with high sensitivity, highly reproducible, reliable and accurate for the content determination of hyodeoxycholic acid in artificial calculus bovis.更多还原