目的 建立高效液相色谱串联质谱同时测定柴胡配方颗粒中柴胡皂苷a、b1、b2、c的含量,为其质量标准的研究提供依据。方法 采用Kinetex C18色谱柱(2.1 mm×100 mm,2.6 μm);流动相为乙腈-0.1%甲酸水溶液,梯度洗脱;流速为300 μL·min-1;柱温40 ℃;质谱条件:采用电喷雾离子源负离子模式进行检测,多反应监测模式(MRM)用于定量测定,源喷射电压为-4 500 V,离子源温度为550 ℃。结果 柴胡皂苷a、b1、b2、c的峰面积与质量浓度在测定范围内均呈良好的线性关系,r≥0.999 1;平均加样回收率分别为100.56%、98.50%、97.44%、99.12%。结论 该方法同时测定了柴胡配方颗粒中柴胡皂苷a、b1、b2、c的含量,方法可行,重现性好,可为柴胡配方颗粒的质量控制提供方法参考。
Abstract
OBJECTIVE To establish a method for determining the contents of saikosaponin a, b1, b2 and c in Radix Bupleuri formula granules by HPLC-MS/MS, and provide scientific basis for the quality standards. METHODS The samples were separated on a Kinetex C18 column (2.1 mm×100 mm, 2.6 μm) by gradient elution at the flow rate of 300 μL·min-1 using acetonitrile and 0.1% aqueous formic acid as the mobile phase. The column temperature was maitained at 40 ℃. Multiple reaction monitoring scanning (MRM) was employed for the quantification with switching electrospray ion source polarity in negative mode. The ion spray voltage was set at -4 500 V and the turbo spray temperature was maintained at 550 ℃. RESULTS There was significant correlation between the peak area and concentration of each compound within the test range (r≥0.999 1). The average recoveries were from 97.44% to 100.56%. CONCLUSION Saikosaponin a, b1, b2 and c are determined by this method simultaneously. The method is available with good reproducibility and can control the quality of Radix Bupleuri formula granules effectively.
关键词
柴胡 /
配方颗粒 /
液质联用 /
柴胡皂苷
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Key words
Radix Bupleuri /
formula granule /
HPLC-MS/MS /
saikosaponin
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中图分类号：
R284
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参考文献
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