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, 5 μm);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1.0 mL·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·mL-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。
Abstract
OBJECTIVE To establish an HPLC-ELSD method for simultaneous quantification of the major bile acids in bear bile powder in its quality assessment and control. METHODS The chromatographic separation was carried out on Agilent SB-C18 column (4.6 mm×250 mm, 5 μm) at 40 ℃ using 10 mmol·L-1 ammonium acetate solution and acetonitrile as the mobile phase at a flow rate of 1.0 mL·min-1. The detection was performed using evaporative light scattering detector at drift tube temperature of 110 ℃ and nitrogen flow rate of 2.8 L·h-1 with 1 as the gain. RESULTS The standard curves of tauroursodeoxycholic acid and taurochenodeoxycholic acid showed good relationship in the ranges of 0.087 2-0.348 8 and 0.076 0-0.342 0 mg·mL-1, respectively. The average recoveries were 101.9% (RSD was 1.9%) and 102.2% (RSD was 1.5%), respectively. CONCLUSION The method is simple, rapid, and accurate. The analysis of the result showed that the method could be used i the quality assessment and control of bear bile powder.
关键词
熊胆粉 /
高效液相色谱法 /
蒸发光散射检测器 /
胆汁酸 /
质量评价 /
质量控制
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Key words
bear bile powder /
HPLC /
ELSD /
bile acid /
quality assessment /
quality control
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中图分类号：
R917
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参考文献
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脚注
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基金
国家十二五“重大新药创制”专项课题——中药质量安全检测和风险控制技术平台(2014ZX09304307-002)
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