UPLC-MS/MS法同时测定排石合剂中10个特征成分含量  

Simultaneous determination of 10 representative components in Paishi mixture by UPLC/MS/MS

作　　者：李均艳 李舒琪 刘辉[1] 王芝燕 何一琴 刘永利 LI Jun-yan;LI Shu-qi;LIU Hui;WANG Zhi-yan;HE Yi-qin;LIU Yong-li(Wujin Traditional Chinese Medicine Hospital of Changzhou City,Jiangsu 213161,China;Hebei University of Chinese Medicine,Shijiazhuang 050020,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China)

机构地区：[1]常州市武进中医医院,常州213161 [2]河北中医药大学,石家庄050020 [3]河北省药品医疗器械检验研究院,石家庄050227

出　　处：《药物分析杂志》2023年第12期2090-2097,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：常州医院协会-常州四药医院药学科研基金CJ20229003。

摘　　要：目的:建立UPLC-MS/MS法同时测定排石合剂中京尼平苷酸、羟基红花黄色素A、绿原酸、苦杏仁苷、王不留行黄酮苷、甘草苷、毛蕊花糖苷、杯苋甾酮、丹皮酚、甘草酸铵10个特征成分的含量。方法:供试品经70%甲醇超声处理,Waters HSS T3 C_(18)(100 mm×2.1 mm,1.7μm)色谱柱,以乙腈-0.1%甲酸为流动相进行梯度洗脱,流速0.3 mL·min^(-1);电喷雾正负离子源同时监测,多反应监测(MRM)模式。结果:方法重复性、准确度良好,10个成分的平均回收率在99.0%~101.0%,RSD为0.090%~4.3%,在各自浓度范围内线性关系良好,含量结果分别为31.129~34.256、95.456~98.741、126.85~129.43、238.62~240.90、45.620~47.520、26.124~28.412、13.852~15.030、16.632~17.854、800.41~805.56、78.485~80.963μg·mL^(-1)。结论:本研究建立的方法快速简便,选择性好,准确可靠,为排石合剂的质量控制提供科学依据。Objective:To establish simultaneous determination method of 10 representative components in Paishi mixture,including geniposidic acid,hydroxyl-safflor yellow A,chlorogenic acid,amygdalin,vaccarin,liquiritin,mulberry glycoside,cyclamenone,paeonol and ammonium glycyrrhizinate.Methods:The sample was ultrasonicated with 70%methanol.The chromatographic separation was performed on a Waters HSS T3 C_(18)(100 mm×2.1 mm,1.7μm)column with acetonitrile-0.1%formic acid solution as mobile phase with gradient elution.The flow rate was 0.3 mL·min^(-1).The analytes were detected by tandem mass spectrometry under the positive and negative ion modes with the ESI source and multiple reaction monitoring(MRM)mode.Results:The repeatability and accuracy of the method were good,and the average recoveries were 99.0%-101.0%with RSDs of0.090%-4.3%.The sample determination results showed that there were differences in the consistency between batches of preparations.The contents of 10 components were 31.129-34.256,95.456-98.741,126.85-129.43,238.62-240.90,45.620-47.520,26.124-28.412,13.852-15.030,16.632-17.854,800.41-805.56,78.485-80.963μg·mL^(-1).Conclusion:The developed method is simple,rapid and accurate,which provides a more comprehensive scientific basis for the quality evaluation of Kechuan mixture.

关 键 词：排石合剂 京尼平苷酸 羟基红花黄色素A 绿原酸 苦杏仁苷 王不留行黄酮苷 甘草苷 毛蕊花糖苷 杯苋甾酮 丹皮酚 甘草酸铵 含量测定 液相色谱质谱联用法 多反应监测 质量控制 

分 类 号：R917[医药卫生—药物分析学]