目的 对蛇胆及其他动物胆中胆汁酸成分进行研究,建立蛇胆药材及其成方制剂的质量控制方法。方法 以乙腈-甲醇及10 mmol·L-1乙酸铵为流动相体系进行梯度洗脱,以十八烷基硅烷键合硅胶为填充剂,采用液相色谱质谱联用技术对蛇胆及其他动物胆中胆汁酸成分进行定性鉴别及定量分析,通过胆汁酸的成分分析结果对蛇胆药材及其成方制剂中蛇胆的检查及含量测定方法进行优化,建立适合的质量控制方法。结果 建立的检查方法专属性强,含量测定方法适宜,牛磺胆酸钠在0.302~9.053 μg之间线性关系良好,r=0.999 3,重复性实验及准确度实验结果良好,RSD均＜3.0%,适合蛇胆药材及其成方制剂的质量控制。结论 建立的质量控制方法能够安全、有效的保证蛇胆药材及其成方制剂的质量,保证用药安全。
Abstract
OBJECTIVE To study the bile acid components in snake bile and other animal bile, and establish the quality control method of the snake bile and its preparations. METHODS Acetonitrile-methanol and 10 mmol·L-1 ammonium acetate was used as mobile phase system and 18 alkyl silane bonded silica gel was used as filling agent. Liquid chromatography-mass spectrometry was used to qualitatively identify and quantitatively analyze the bile acid components in snake bile and other animal bile, and the adulteration control and content determination method of bile acid in snake bile and its preparations were optimized to establish a suitable quality control method of snake bile and its preparations. RESULTS The examination method was highly specialized and suitable for the quality control of snake bile and its preparations.The linear relationship of sodium taurocholate between 0.302-9.053 μg is good, r=0.999 3, the repeatability test and accuracy test results are good, and the RSD is smaller than 3.0%. CONCLUSION The established quality control method can guarantee the quality and safety of snake bile and its preparations.
关键词
蛇胆 /
蛇胆成方制剂 /
胆酸类成分 /
掺伪检查 /
含量测定
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Key words
snake bile /
snake bile preparation /
bile acid /
adulteration control /
content determination
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中图分类号：
R284
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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”专项资助(2014ZX09304307-002);国家自然科学基金面上项目资助(81274025)
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