柱前衍生化高效液相色谱法测定清开消炎片中猪去氧胆酸的含量

目的建立柱前衍生化高效液相色谱法测定清开消炎片中猪去氧胆酸含量。方法以0.1%18-冠醚-6乙腈溶液为催化剂,0.6%1-溴乙酰基对硝基苯乙腈溶液对清开消炎片中的猪去氧胆酸进行衍生化,采用高效液相色谱法测定;以Waters Symmetry 5C1(8250mm×4.6mm,5μm)为色谱柱;流动相:乙腈-水(60:40);流速:1.0mL·min-1;柱温:35℃;检测波长:254nm。结果空白无干扰,线性关系良好。结论该方法简便、快捷、重复性好,能准确测定清开消炎片中猪去氧胆酸的含量,为清开消炎片的质量控制提供了依据。

Determination of Hyodeoxycholic Acid in Qingkai Xiaoyan Tablets by Pre-Column Derivatization HPLC

Objective To establish an pre -column derivation HPLC method for the determination of hyodeoxycholic acid in Qingkai Xiaoyan Tablets. Methods After With 0.1 % 18-crown ether-6-acetonitrile as the catalyst, thed-erivation of hyodeoxycholic acid was induced by 0.6 % 1-(2-bromoacetyl)-p-nitophenylacetonitrile. After derivation, the sample was separated at 35 ℃ on a Waters Symmetry~(R) 5C_(18) (250 mm × 4.6 mm, 5 μm) eluted with acetonitrile and water (60 : 40). The detection wavelength was 254 nm, and the velocity of flow was 1.0 mL·min~(-1). Results The compound was resolved and the negative sample showed no interference, and the linear relationship of hyodeoxycholic acid was excellent. Conclusion The method was simple, rapid, precise and with good reproducibility. This method can be uses to detect the content of hyodeoxycholic acid in Qingkai Xiaoyan Tablets.