Rapid and sensitive liquid chromatography with tandem mass spectrometry method for the simultaneous determination of 11 major components of Yuanhu-Baizhi herb-pair in rat perfusion fluids.
Rapid and sensitive liquid chromatography with tandem mass spectrometry method for the simultaneous determination of 11 major components of Yuanhu-Baizhi herb-pair in rat perfusion fluids.
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DOI：
10.1002/jssc.201400054
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发表时间：
2014-06
影响因子：
3.1
通讯作者：
Yinli Liu;Bin Chen;Jian Le;Yanhai Xu;Lin Song;Y. Chai;Guorong Fan;Z. Hong
中科院分区：
文献类型：
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作者：
Yinli Liu;Bin Chen;Jian Le;Yanhai Xu;Lin Song;Y. Chai;Guorong Fan;Z. Hong
建立了一种快速、灵敏的液相色谱-串联质谱法（LC-MS-MS），并以地西泮为内标，对元胡-八芝药对中的11种主要成分进行了定量分析。在Agilent Poroshell 120 EC-C18柱上进行分析，使用乙腈/H2 O（含0.0015%甲酸和2 mM甲酸铵缓冲液添加剂（pH 4.2））梯度洗脱。所有化合物均通过串联质谱法以正离子模式检测，并使用多反应监测模式进行定量。在各化合物的相关范围内呈现良好的线性。验证数据（如准确度和精密度）均在要求的限度内。每种分析物的定量下限均小于10 ng/mL。日内和日间精密度均小于12.84%。准确度的相对误差在-13.31 ~13.19%之间。回收率均大于84.08%。该方法已成功地应用于元胡-八芝药对提取物大鼠肠灌流后主要成分的肠吸收研究。
A rapid and sensitive liquid chromatography with tandem mass spectrometry method has been developed and validated for the simultaneous quantification of 11 major compounds in Yuanhu-Bazhi herb-pair from a rat intestinal perfusion experiment, including eight alkaloids and three coumarins using diazepam as the internal standard. The analysis was performed on an Agilent Poroshell 120EC-C18 column using a gradient elution of acetonitrile/H2 O with 0.0015% formic acid and 2 mM ammonium formate buffer additive (pH 4.2). All compounds were detected by tandem mass spectrometry in positive ionization mode and quantified using multiple reaction monitoring mode. Good linearity in the related range of each compound was presented. The validation data, such as accuracy and precision, were within the required limits. The lower limit of quantification of each analyte was less than 10 ng/mL. Intra-day and inter-day precisions were less than 12.84%. The relative errors of accuracy were in the range of -13.31 to 13.19%. The recoveries of analytes were greater than 84.08%. The method has been successfully applied to an intestinal absorption study of major components following intestinal perfusion of Yuanhu-Bazhi herb-pair extract to rats.