论文部分内容阅读
目的采用RP-HPLC法测定牛磺熊去氧胆酸胶囊中的有关物质。方法采用Diamonsil C18色谱柱(150 mm×4.6mm,5μm),流动相为0.02 mol.L-1磷酸二氢钠-乙腈(60∶40,磷酸调pH5.5),检测波长为205 nm,流速为1.0 mL.min-1,柱温30℃。结果牛磺熊去氧胆酸0.9694～96.94μg.mL-1与峰面积的线性关系良好(r=0.9999),检测限为0.3635 ng,定量限为1.454 ng。牛磺鹅去氧胆酸0.9443～94.43μg.mL-1与峰面积的线性关系良好(r=0.9999),检测限为9.447 ng,定量限为23.62 ng,方法回收率为99.54%。结论所用方法准确、灵敏、快速,适用于牛磺熊去氧胆酸胶囊中微量杂质的控制。
Objective To determine the related substances in tauroursodeoxycholic acid capsules by RP-HPLC. Methods Diamonsil C18 column (150 mm × 4.6 mm, 5 μm) was used. The mobile phase consisted of 0.02 mol·L -1 sodium dihydrogen phosphate - acetonitrile (60:40, pH5.5 adjusted by phosphoric acid). The detection wavelength was 205 nm, 1.0 mL.min-1, column temperature 30 ℃. Results The linear relationship between the concentration of tauroursodeoxycholic acid and the peak area was 0.9694 ~ 96.94μg.mL-1 (r = 0.9999). The detection limit was 0.3635 ng and the limit of quantification was 1.454 ng. The linear range of 0.9443 ~ 94.43μg.mL-1 for taurochenodeoxycholic acid was good (r = 0.9999), the detection limit was 9.447 ng, the limit of quantification was 23.62 ng, and the recovery rate was 99.54%. Conclusion The method is accurate, sensitive and rapid and suitable for the control of trace impurities in tauroursodeoxycholic acid capsules.