基于UPLC-MS/MS分析法同时测定健脾解毒方6种活性成分含量

Simultaneous determination of 6 components in Jianpi Jiedu by UPLC-MS/MS

目的建立同时测定健脾解毒方中原儿茶酸、毛蕊异黄酮葡萄糖苷、人参皂苷Re、人参皂苷Rb1、芹菜素、异甘草素6种成分的UPLC-MS/MS分析方法,并对健脾解毒方中上述成分进行检测。方法采用液质联用方法,应用Poroshell 120 SB-Aq（50 mm×2.1 mm,1.7μm）色谱柱,流动相为0.1%甲酸的水溶液和0.1%乙腈溶液梯度洗脱,采用电喷雾电离源（ESI）,多反应离子监测（MRM）扫描方式进行检测。结果健脾解毒方中6种成分线性关系、精密度、稳定性、重复性均符合方法学测定要求,加样回收率为95.2%~102.6%。利用建立的方法测定了6批次健脾解毒方中原儿茶酸等6个成分含量。结论利用建立的方法同时测定健脾解毒方中6种成分的方法具有操作简单、重复性好、准确可靠,可为健脾解毒方质量控制提供依据。

Objective To establish an UPLC-MS/MS method for simultaneous determination of protocatechuic acid, calycosin-7-glucoside, ginsenoside-Re, ginsenoside Rb1, apigenin and isoliquiritigenin in Jianpi Jiedu（JPJD）, and measured the content of these components in JPJD. Methods The 6 components in JPJD was quantitatively studied by UPLC-MS/MS on a Poroshell 120 SB-Aq（50 mm×2.1 mm, 1.7 μm） column with a gradient elution（0.1% formic acid aqueous solution and 0.1% acetonitrile solution）. A triple quadrupole mass spectrometer operating in electrospray ionization mode with multiple reaction monitoring was used. Results The 6 components in JPJD had good linearity, precision, stability, and repeatability according to the requirements of the methodology determination. The recoveries were 95.2%- 102.6%. The 6 components in 6 batches of JPJD were determined by UPLC-MS/MS. Conclusion The developed UPLC-MS/MS method is simple, sensitive, accurate, and repeatable. The 6 components in JPJD can be rapidly, accurately and quantitatively analyzed by UPLC-MS/MS, which provides helpful information for the comprehensive quality evaluation of JPJD.