基于UPLC-MS/MS同时定量分析半夏不同炮制品中8种潜在毒性成分

Simultaneous Quantitative Analysis of 8 Potential Toxic Components in Different Processed Products of Pinellia ternata Based on UPLC-MS/MS

[目的]建立超高效液相串联质谱(UPLC-MS/MS)法同时测定半夏生品及其炮制品中8种潜在毒性成分的含量,并分析其潜在毒性成分的差异。[方法]采用UPLC-MS/MS法测定半夏生品及其炮制品中8种潜在毒性成分的含量并进行方法学考察。流动相为甲醇-水溶液,梯度洗脱,流速为0.3 mL/min,质谱离子源为电喷雾离子源(ESI),检测模式为多反应监测(MRM),以苦参碱(正离子)和野黄芩苷(负离子)作为内标物。采用多元统计分析方法对8种潜在毒性成分的含量与炮制方法的相关性进行评价。[结果]8种潜在毒性成分在各自范围内线性关系良好(R^(2)≥0.999)。经多元统计分析,样品被聚集为4类,并通过变量权重重要性排序(VIP)发现胆碱、盐酸麻黄碱和原儿茶酸为4类样品间的主要差异成分。[结论]该方法快速、准确、灵敏度高、重现性好,可用于半夏生品及其炮制品中8种潜在毒性成分的含量测定,为后续分析提供参考。

[Objective]To establish an ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the simultaneous determination of eight potentially toxic components in Pinellia ternata and its processed products,and to analyze the differences of their potentially toxic components.[Method]The UPLC-MS/MS method was used to determine 8 poential toxic components in different processed products of Pinellia ternata and to conduct a methodological investigation.The mobile phase was methanol-water solution,gradient elution,flow rate was 0.3 mL/min,mass spectrometry ion source was electrospray ionization source(ESI),detection mode was multiple reaction monitoring(MRM),matrine(positive ion)and scutellarin(negative ion)was used as the internal standard.The multivariate statistical analysis method was used to evaluate the correlation between the contents of the 8 toxic components and the processing methods.[Results]The 8 poential toxic components had a good linear relationship within their respective ranges(R^(2)≥0.999).After multivariate statistical analysis,the samples were clustered into 4 categories,and through variable weighted importance ranking(VIP),choline,ephedrine hydrochloride and protocatechuic acid were found to be the main differences among the 4 types of samples.[Conclusion]The method is rapid,accurate,sensitive and reproducible.It can be used for the determination of 8 potential toxic components in Pinellia ternata and its processed products,and provide reference for subsequent analysis.