·74·江西中医药大学学报2023年8月第35卷第4期JOURNALOFJIANGXIUNIVERSITYOFCM2023Vol.35No.4●中药研究●UPLC-MS/MS法测定右归丸中毛蕊花糖苷的含量★邓杰华1周云峰1黄招光1吴喆1黄炳泉1李存金2(1.宜春市检验检测中心江西宜春336000;2.江西省药品检查员中心南昌330029)[摘要]目的:建立右归丸中毛蕊花糖苷的含量测定方法。方法:采用WatersACQUITYUPLCBEHC18色谱柱(2.1mm×100mm,1.7μm),以乙腈-0.1%甲酸溶液为流动相,梯度洗脱,流速0.3mL/min,柱温30℃;质谱条件以623→161和623→133为特征离子对,采用电喷雾离子源(ESI)和负离子扫描方式,进行多反应离子监测(MRM)定量分析。结果:毛蕊花糖苷在质量浓度175.7392~1757.3920ng/mL范围内呈良好线性关系,方法学考察良好。9批样品中毛蕊花糖苷的含量范围为33.40~53.20μg/g。结论:所建方法能测定右归丸中熟地黄的主要化学成分的含量,可用于右归丸的质量控制。[关键词]右归丸;熟地黄;毛蕊花糖苷;液质联用;含量中图分类号:R284.1文献标志码:ATheContentDeterminationofVerbascosideinYouguiPillsbyUPLC-MS/MSDENGJie-hua1,ZHOUYun-feng1,HUANGZhao-guang1,WUZhe1,HUANGBing-quan1,LICun-jin21.YichunInspectionandTestingCenter,Yichun336000,China;2.JiangxiDrugInspectionCenter,Nanchang330029,China.[Abstract]Objective:ToestablishamethodforthecontentdeterminationofverbascosideinYouguipills.Methods:Theliquidchromatographywasperformedusingacetonitrile-0.1%formicacidasmobilephaseingradientelutionataflowrateof0.3mL/minandcolumntemperatureof30℃.Themassspectrometryconditionswerecharacterizedbyionpairs623→161and623→133,electrosprayionsourceandpositiveionscanning,andmultiplereactiveionmonitoring(MRM)quantitativeanalysis.Results:Agoodlinearrelationshipwasfoundinthemassconcentrationrangeof175.7392-1757.3920ng/mL.Thecontentofverbascosidein9batchesofsamplesrangedfrom33.40μg/gto53.20μg/g.Conclusion:ThemethodcanbeusedtodeterminethecontentofmainchemicalcomponentsofRadixrehmanniaepraeparatainYouguipillsandtocontrolthequalityofYouguipills.[Keywords]YouguiPills;RadixRehmanniaePraeparata;Verbascoside;UPLC-MS;Content基金项目:江西省药品监督管理局科研项目(2019JS24)。通信作者:李存金,副主任药师。E...