UPLC-ESI-MS法分析盆炎清栓主要成分

Analysis of main components in Penyanqing Suppository by UPLC-ESI-MS

目的建立UPLC-ESI-MS法分析盆炎清栓(吲哚美辛、毛冬青提取物)主要成分。方法该药物甲醇提取液的分析采用Waters Acauity UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm);流动相乙腈(含0.1%甲酸)-水(含0.1%甲酸),梯度洗脱;体积流量0.4 mL/min;柱温40℃;电喷雾电离源;负离子模式。测定指标成分(芦丁、冬青苷O、毛冬青皂苷B 3、毛冬青皂苷B 2、毛冬青皂苷A 1、毛冬青皂苷B 1、吲哚美辛、冬青素A)的含量。结果共鉴定出91个化合物,包括54个三萜、22个苯丙素、9个黄酮、6个其他化合物,并验证37个化合物的结构。8种指标成分在各自范围内线性关系良好(R^(2)≥0.9990),平均加样回收率97.84%~103.04%,RSD 1.22%~3.39%。结论该方法稳定可靠,可用于盆炎清栓的质量控制。

AIM To establish a UPLC-ESI-MS method for the analysis of main components in Penyanqing Suppository(indomethacin,extract of Ilex pubescens Hook.et Arn.).METHODS The analysis of methanol extract of this drug was performed on a 40℃thermostatic Waters Acauity UPLC HSS T3 column(100 mm×2.1 mm,1.8μm),with the mobile phase comprising of acetonitrile(containing 0.1%formic acid)-water(containing 0.1%formic acid)flowing at 0.4 mL/min in a gradient elution manner,and electrospray ionization source was adopted in negative mode.The contents of index components(rutin,ilexoside O,ilexsaponin B_(3),ilexsaponin B_(2),ilexsaponin A_(1),ilexsaponin B_(1),indomethacin and ilexgenin A)were determined.RESULTS Total 91 compounds were identified,containing 54 triterpenes,22 phenylpropanoids,9 flavones and 6 other compounds,and the structures of 37 compounds were confirmed.Eight index components showed good linear relationships within their own ranges(R≥0.9990),whose average recoveries were 97.84%-103.04%with the RSDs of 1.22%-3.39%.CONCLUSION This stable.and reliable method can be used for the quality control of Penyanqing Suppository.