UPLC-MS/MS法同时测定熟附片中6种生物碱类成分含量

Simultaneous Determination of Six Alkaloids in Shufupian by UPLC-MS/MS

目的建立超高效液相色谱串联质谱(UPLC-MS/MS)法同时测定熟附片中6种生物碱类成分的含量。方法UPLC分析采用Waters UPLC HSS C18色谱柱(2.1 mm×100 mm,1.8μm);流动相为乙腈和0.1%甲酸溶液,采用梯度洗脱,进样量为1μL,柱温为40℃,流速为0.2 mL/min。质谱系统定量测定采用多反应监测模式(MRM),检测模式采用电喷雾离子源正离子(ESI^(+))。结果在考察浓度线性范围内6种生物碱类成分的线性关系良好,r值均大于0.999;回收率和RSD分别在96.54%~103.60%和0.69%~1.89%之间。结论UPLC-MS/MS能同时、快速、准确地检测熟附片中6种生物碱类成分的含量,重现性好,可为熟附片的质量控制提供参考。

Objective To establish a determination of six alkaloids in shufupian by using UPLC-MS/MS.Methods Waters UPLC HSS C18 column(2.1 mm×100 mm,1.8μm)was used for UPLC analysis.The mobile phase consisted of acetonitrile and 0.1%formic acid solution with gradient elution.The sample size was 1μL,the column temperature was 40℃,and the flow rate was 0.2 mL/min.Multiple reaction monitoring mode(MRM)and electrospray ion source positive ion(ESI^(+))were used for quantitative determination in mass spectrometry system.Results Six alkaloids showed good linear relationships within their own ranges,and the r value was greater than 0.999,the overall recoveries were ranged from 96.54%-103.60%with the RSD from 0.69%-1.89%.Conclusion The developed method is feasible and reproducible which can be used for the quality control of shufupian.