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目的建立适用于对熊胆粉进行质量评价与控制的主要胆汁酸类成分的HPLC-ELSD测定方法。方法使用Agilent SB-C18色谱柱(4.6 mm×250 mm,5μm);柱温为40℃,10 mmol·L~(-1)乙酸铵水溶液和乙腈作为流动相,梯度洗脱,流速1.0m L·min~(-1);ELSD漂移管温度为110℃,ELSD氮气流速为2.8 L·h~(-1),增益为1。结果牛磺熊去氧胆酸、牛磺鹅去氧胆酸的进样量对数值与峰面积对数值分别在0.087 2~0.348 8和0.076 0~0.342 0 mg·m L~(-1)内呈良好的线性关系;平均回收率分别为101.9%和102.2%,RSD值分别为1.9%和1.5%。结论所建立的方法简便、快捷、准确,对结果分析显示该法适用于熊胆粉的质量评价与控制。
OBJECTIVE To establish a HPLC-ELSD method for the determination of main bile acids in bear dander powder for quality evaluation and control. Methods The Agilent SB-C18 column (4.6 mm × 250 mm, 5 μm) was used. The column temperature was 40 ℃, 10 mmol·L -1 ammonium acetate aqueous solution and acetonitrile were used as the mobile phase. · Min ~ (-1). The ELSD drift tube temperature was 110 ℃, and the flow rate of ELSD nitrogen gas was 2.8 L · h -1 with a gain of 1. Results The logarithm and peak area values of tauroursodeoxycholic acid and tauroursodeoxycholic acid were 0.087 2 ~ 0.348 8 and 0.076 0 ~ 0.342 0 mg · m L -1, respectively The average recoveries were 101.9% and 102.2%, respectively, with RSDs of 1.9% and 1.5%, respectively. Conclusion The established method is simple, rapid and accurate. Analysis of the results shows that the method is suitable for the quality evaluation and control of bear gall powder.