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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
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金高娃,宋春颖,闫竞宇,刘艳芳,沈爱金,郭志谋,梁鑫淼 1.中国科学院大连化学物理研究所中国科学院分离分析化学重点实验室2. 中国科学院大连化学物理研究所-中国医药城生物医药创新研究院 
基金项目:国家自然科学基金重点项目(U1508221)
中文摘要: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,1.7 μm)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。
中文关键词:舒血宁注射剂  超高效液相色谱-串联质谱  黄酮苷类  萜类内酯  同时定量分析
 
Simultaneous Determination of 20 Flavonoid Glycosides and Terpenoid Lactones in Shuxuening Injection by Ultra-high Performance Liquid Chromatography-Mass Spectrometry
Abstract: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(1.7 μm,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(r2) no less than 0.963 3.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.
Key Words:shuxuening injection  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  flavonoid glycosides  terpenoid lactones  simultaneous quantitative analysis
引用本文:金高娃,宋春颖,闫竞宇,刘艳芳,沈爱金,郭志谋,梁鑫淼.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[J].分析测试学报,2020,39(1):115-121.
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