UPLC-MS/MS法测定心可舒胶囊中木香烃内酯与去氢木香内酯的含量

Content Determination of Covanolactone and Dehydrocovanolactone in Xinkeshu Capsules by UPLC-MS/MS

目的 建立超高效液相色谱串联质谱法(UPLC-MS/MS)测定心可舒胶囊中木香烃内酯与去氢木香内酯的含量。方法 以Waters ACQUITY UPLC?BEH C18(1.7μm×2.1 mm×100 mm)为色谱柱,流动相为0.1%甲酸-乙腈(梯度洗脱),流速为0.3 ml/min,柱温35℃,进样量2μl;质谱采用电喷雾离子源(ESI)、正离子扫描模式,以多反应监测模式(MRM)进行数据采集,木香烃内酯的定量离子对为m/z 233→187,去氢木香内酯的定量离子对为m/z 231→185。结果 木香烃内酯与去氢木香内酯分别在0.0430~2.1498μg/ml、0.0439~2.1970μg/ml浓度范围内线性关系良好(r≥0.9913),平均加标回收率为102.60%和95.56%,RSD分别为3.6%与2.3%。3批样品木香烃内酯的含量范围为5.267~5.574 mg/g,去氢木香内酯的含量范围为4.822~5.191 mg/g。结论 所建方法能有效测定心可舒胶囊中木香烃内酯与去氢木香内酯的含量,可为完善该制剂的质量标准提供借鉴。

Objective In order to establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for the determination of costunolide and dehydrocosinolactone in Xinkeshu capsules.Methods The determination was performed on a Waters ACQUITY UPLC®BEH C18(1.7μm×2.1 mm×100 mm)column with mobile phase consisted of 0.1%formic acid-acetonitrile(gradient elution)at the flow rate of 0.3 ml/min.The column temperature was35℃,and sample size was2μl.The mass spectrometry was performed using ESI and positive ion scanning mode,and multi-reaction monitoring mode(MRM).Quantitative ion pairs of costunolide were m/z 233→187,and quantitative ion pairs of dehydrocodenolactone were m/z 231→185.Results The linear range of costunolide and dehydrocostinolactone was 0.0430~2.1498μg/ml and 0.0439~2.1970μg/ml respectively(r≥0.9913).The average recoveries were 102.60%and 95.56%,RSDS were 3.6%and 2.3%,respectively.The contents of costunolide and dehydrocosinolactone in three batches of samples ranged from 5.267 to 5.574 mg/g and 4.822 to 5.191 mg/g.Conclusion The established method can effectively determine the contents of costunolide and dehydrocovanolactone in Xinkeshu capsules,and can provide reference for improving the quality standard of this preparation.