超高效液相色谱-质谱法同时测定舒血宁注射剂中20种黄酮醇苷与萜类内酯成分

Simultaneous Determination of 20 Flavonoid Glycosides and Terpenoid Lactones in Shuxuening Injection by Ultra-high Performance Liquid Chromatography-Mass Spectrometry

建立了舒血宁注射剂中16种黄酮及4种萜类内酯同时定量的超高效液相色谱-质谱分析方法,并采用所建立的方法同时测定了不同厂家舒血宁注射剂产品中上述20种化合物的含量。注射剂样品经甲醇-水(体积比1∶1)稀释后,在Acquity UPLC BEH Shield RP18(2.1 mm×100 mm,1.7μm)色谱柱上分析,以0.1%(体积分数)甲酸水溶液-乙腈为流动相进行梯度洗脱,以电喷雾离子源负离子多反应监测(MRM)模式进行质谱监测。结果表明:20种化合物可在10 min内完成色谱分离分析,检出限和定量下限分别为0.02~1.59 ng/mL和0.07~5.30 ng/mL,16种黄酮及4种萜类内酯在各自的线性范围内线性关系良好,在低、中、高3个加标水平下的回收率为85.9%~109%。该方法前处理简单、快速高效、准确性高,为舒血宁注射剂的质量控制提供了参考。

A method of ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was developed for the simultaneous determination of 16 flavonoid glycosides and 4 terpenoid lactones in shuxuening injections.The samples were firstly diluted with methanol-water(1%1,by volume),and then separated on an ACQUITY UPLC BEH Shield RP18 column(1.7μm,2.1 mm×100 mm)by gradient elution using acetonitrile-water containing 0.1%formic acid as mobile phases,finally detected by UPLC-MS/MS with ESI source in MRM mode.Results revealed that the 20 compounds could be analyzed within 10 min.There were good linear relationships for twenty compounds in a certain concentration range with their correlation coefficients(r^2)no less than 0.9633.The limits of detection(LODs)and limits of quantitation(LOQs)were in the ranges of 0.02-1.59 ng/mL and 0.07-5.30 ng/mL,respectively.And the recoveries at three levels were between 85.9-109%.This method was applied in the simultaneous detection of 16 flavonoid glycosides and 4 terpenoid lactones in different shuxuening injection products.With the advantages of simplicity,rapidness and good repeatability,the method is suitable for the quantitative analysis of 20 compounds in shuxuening injections,and provides a good strategy for further quality control of shuxuening injections.