UPLC-MS/MS同时测定麦冬配方颗粒中4个成分的含量及山麦冬成分的检查  

Simultaneous Determination of Four Components in Ophiopogon Japonicus Formula Granules by UPLC-MS/MS and Inspection of ingredients of Liriopes Radix

作　　者：刘斌 张力伟 王煦辰 孔令红 赵海燕 周海燕 丁富娟 LIU Bin;ZHANG Li-wei;WANG Xu-chen;KONG Ling-hong;ZHAO Hai-yan;ZHOU Hai-yan;DING Fu-juan(Taian Testing Institute for Food and Drug Control,Taian 271000,China;Daiyue District Center for Disease Control and Prevention,Taian 271000,China)

机构地区：[1]泰安市食品药品检验检测研究院,山东泰安271000 [2]泰安市岱岳区疾病预防控制中心,山东泰安271000

出　　处：《中国现代中药》2024年第1期144-151,共8页Modern Chinese Medicine

基　　金：山东省2022年药品质量安全风险监测项目。

摘　　要：目的:采用超高效液相色谱-三重四极杆串联质谱法(UPLC-MS/MS)建立同时测定麦冬配方颗粒中4个有效成分的含量,并检查是否含有山麦冬的2个专属性成分的方法。方法:采用XBridge BEH C18色谱柱(100 mm×2.1 mm,2.5μm),流动相为乙腈(A)-0.1%甲酸水溶液(B),梯度洗脱,流速:0.2 mL·min^(–1),柱温:35℃,电喷雾离子源,多反应监测模式正、负离子全扫描。对麦冬配方颗粒中麦冬皂苷C、麦冬皂苷D、甲基麦冬黄烷酮A、甲基麦冬黄烷酮B、山麦冬皂苷B、短葶山麦冬皂苷C进行含量测定并聚类分析。结果:6个待测成分在各自线性范围内线性关系良好(r≥0.995),平均加样回收率为95.9%~99.3%,RSD为0.9%~2.2%。26批样品中麦冬皂苷C、麦冬皂苷D、甲基麦冬黄烷酮A、甲基麦冬黄烷酮B的质量分数分别为6.4~17.3、15.1~29.1、9.0~22.6、4.5~14.4μg·g–1;有3批检出山麦冬皂苷B,其中2批同时检出短葶山麦冬皂苷C。结论:该方法简单、快速、准确,可用于麦冬配方颗粒的质量控制。Objective:An ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to simultaneously determine four active components in Ophiopogon japonicus Formula Granules and detect the two specific components of Liriopes Radix.Methods:The XBridge BEH C18 chromatographic column(100 mm×2.1 mm,2.5μm)was used.With acetonitrile(A)-0.1%formic acid aqueous solution(B)as mobile phase,gradient elution was performed.The flow rate was 0.2 mL·min^(-1),and the column temperature was set at 35°C.Electro spray ion source(ESI)and full scanning of positive and negative ions in multi-reaction monitoring(MRM)mode were conducted.The content of ophiopogon saponin C,ophiopogon saponin D,methylophiopogonanone A,methylophiopogonanone B,liriopeside B,and liriope muscari baily saponin C in Ophiopogon japonicus Formula Granules was determined,and cluster analysis was performed.Results:The six components to be measured had a good linear relationship(r≥0.995)in their respective linear ranges,whose average recoveries were 95.9%-99.3%,with the RSD of 0.9%-2.2%.The content ranges of ophiopogon saponin C,ophiopogon saponin D,Methylophiopogonanone A,and Methylophiopogonanone B in 26 batches of samples were 6.4-17.3,15.1-29.1,9.0-22.6,4.5-14.4μg·g^(-1),respectively.Three batches of samples were detected with liriopeside B,and two batches were detected with liriope muscari baily saponin C.Conclusion:The method is simple,fast,and accurate,which can be used for the quality control of Ophiopogon japonicus Formula Granules.

关 键 词：麦冬配方颗粒 超高效液相色谱-三重四极杆串联质谱法 麦冬皂苷C 麦冬皂苷D 甲基麦冬黄烷酮A 甲基麦冬黄烷酮B 山麦冬皂苷B 短葶山麦冬皂苷C 

分 类 号：R284[医药卫生—中药学]