论文部分内容阅读
目的:建立同时测定猪胆粉药材中牛磺猪胆酸、牛磺猪去氧胆酸和牛磺鹅去氧胆酸含量的RP-HPLC方法。方法:采用Welchrom C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-磷酸二氢钠溶液(0.03 mol·L-1)(70∶30),用磷酸调节pH为4.4,流速为1.0 mL·min-1,检测波长200 nm,柱温25℃。结果:牛磺猪胆酸、牛磺猪去氧胆酸和牛磺鹅去氧胆酸进样量分别在1.65～16.5μg(r=0.9998),2.03～20.3μg(r=0.9998),1.09～10.9μg(r=0.9996)范围内线性关系良好;检测限分别为26.4,7.6,38.2 ng;平均加样回收率(n=9)分别为101.2%(RSD=1.9%),99.1%(RSD=1.7%),100.6%(RSD=2.1%)。结论:该方法简便、准确,重复性好,在同一色谱条件下实现多指标成分的同时测定,为猪胆粉的全面质量评价提供参考。
Objective: To establish an RP-HPLC method for the simultaneous determination of tauroursodeoxycholic acid, tauroursodeoxycholic acid and tauroursodeoxycholic acid in pork gall powder medicine. Methods: The mobile phase consisted of methanol-sodium dihydrogen phosphate solution (0.03 mol·L-1) (70:30) on a Welchrom C18 column (250 mm × 4.6 mm, 5 μm) 1.0 mL · min-1, detection wavelength 200 nm, column temperature 25 ℃. Results: The injection rates of taurocholic acid, taurodeoxycholic acid and taurochenodeoxycholic acid were 1.65-16.5μg (r = 0.9998), 2.03-20.3μg (r = 0.9998), 1.09-10.9μg (r = 0.9996). The detection limits were respectively 26.4, 7.6 and 38.2 ng. The average recoveries were 101.2% (RSD = 1.9%) and 99.1% (RSD = 1.7% ), 100.6% (RSD = 2.1%). Conclusion: The method is simple, accurate and reproducible. Simultaneous determination of multi-index components under the same chromatographic conditions provides a reference for the overall quality evaluation of porcine bile powder.