基于“安全-有效”的清肺排毒颗粒中细辛的薄层色谱鉴别及马兜铃酸Ⅰ的监测研究

Thin-layer Chromatograpnic identification of Asarum and determination of Aristolochic acid Ⅰ in Qingfei Paidu Granules based on"safe-effective"considerations

目的建立清肺排毒颗粒中细辛药材的薄层色谱鉴别方法及马兜铃酸Ⅰ的限量检测方法,进一步完善清肺排毒颗粒的质量控制标准,为企业生产提供依据。方法依据细辛现行质量标准,优化和完善清肺排毒颗粒中细辛药材的薄层鉴别方法。采用Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm)色谱柱,乙腈、水(0.1%甲酸)为流动相,梯度洗脱,流速0.3 mL·min^(-1),柱温35℃。采用三重四级杆质谱检测器,正离子模式下,进行多反应检测。结果薄层色谱分离度良好。马兜铃酸Ⅰ在20.44~204.4 pg(R^(2)=0.9994)线性关系良好,平均回收率为104.85%(RSD=5.45%,n=9)。15批清肺排毒颗粒的马兜铃酸I含量均低于0.25μg·g^(-1),符合标准。结论该研究所建方法简便、灵敏,可用于清肺排毒颗粒的质量控制,有助于细辛质量控制方法的完善和提高,为清肺排毒颗粒的安全使用提供依据。

Objective To provide a basis for further improvement of the quality control standards and enterprise production of Qingfei Paidu Granules(QFPDG),this study established a thin-layer Chromatography(TLC)identification method for the identification of asarum and a method for the determination of aristolochic acid Ⅰ in QFPDG.Methods Based on the current quality standard of asarum,the TLC method of asarum in QFPDG was further optimized and improved.A Waters ACQUITY UPLC HSS T3(2.1 mm×100 mm,1.8μm)column was used,with acetonitrile and water(0.1%formic acid)as mobile phases;flow rate:0.3 mL·min^(-1);column temperature:35℃.A triple quadrupole mass spectrometer detector in positive ion mode was used for multiple reaction monitoring detection.Results The linear range of aristolochic acid Ⅰ was 20.44~204.4 pg(R^(2)=0.9994).The average recovery was 104.85%(RSD=5.45%,n=9).Conclusion The proposed method was simple,sensitive and suitable for the quality control,which would help to improve and refine the quality control method of asarum and provide the basis for the safe use of QFPDG.