摘要
目的建立超高效液相色谱串联质谱法(UPLC-MS/MS)同时测定复方地黄合剂中小檗碱、黄柏碱、特女贞苷、芒果苷、莫诺苷、马钱苷、芍药苷、栀子苷、黄芩苷和毛蕊花糖苷10种成分的含量。方法采用UPLC-MS/MS法,色谱柱为ACQUITY UPLC BEH-C18(2.1 mm×100 mm,1.7μm),流动相为0.1%甲酸水(A)-甲醇(B),梯度洗脱,流速为0.2 ml/min,柱温30℃,进样量2μl。采用多反应离子检测模式(MRM)。结果复方地黄合剂中10种成分在各自浓度范围内线性关系良好,精密度、重复性、稳定性和加样回收率结果均符合要求;7批次样品中小檗碱、黄柏碱、特女贞苷、芒果苷、莫诺苷、马钱苷、芍药苷、栀子苷、黄芩苷和毛蕊花糖苷的含量分别为(89.7~95.6)μg/ml、(164.0~177.7)μg/ml、(540.0~610.0)μg/ml、(408.7~429.0)μg/ml、(726.0~825.0)μg/ml、(503.7~572.0)μg/ml、(1380.0~1540.0)μg/ml、(2596.7~2896.7)μg/ml、(4866.7~5520.0)μg/ml、(61.8~67.2)μg/ml。结论该方法重复性好、操作简便,可快速准确地测定复方地黄合剂中10种成分的含量,并为其质量控制提供参考。
Objective To develop an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method to simultaneously determine 10 main components,including berberine,phellodendrine,specnuezhenide,mangiferin,loganin,paeoniflorin,geniposide,baicalin,and acteoside in Compound Dihuang oral solution.Methods An UPLC-MS/MS method was established with an ACQUITY UPLC BEH-C18(2.1 mm×100 mm,1.7μm)column and mobile phase of 0.1%formic water(A)-methanol solution(B)in a gradient elution manner.The flow rate of mobile phase was 0.2 ml/min.The temperature of column was 30℃.The injection volume was 2μl.The MS detection was in MRM mode.Results 10 components in Compound Dihuang oral solution had a good linear relationship within their concentration range,and the precision,repeatability,stability and recovery met the requirements.The contents of berberine,phellodendrine,specnuezhenide,mangiferin,loganin,paeoniflorin,geniposide,baicalin,and acteoside in 7 batches of samples were(89.7-95.6)μg/ml,(164.0-177.7)μg/ml,(540.0-610.0)μg/ml,(408.7-429.0)μg/ml,(726.0-825.0)μg/ml,(503.7-572.0)μg/ml,(1380.0-1540.0)μg/ml,(2596.7-2896.7)μg/ml,(4866.7-5520.0)μg/ml,(61.8-67.2)μg/ml,respectively.Conclusion The established method was easy to be repeated and operated.The contents of 10 components in Compound Dihuang oral solution could be determined quickly and accurately,which provided a reference for the quality control of hospital preparation.
作者
刘红霞
孙延文
韩菲
周妍
孙华君
丁丽琴
LIU Hongxia;SUN Yanwen;HAN Fei;ZHOU Yan;SUN Huajun;DING Liqin(Department of Pharmacy,Shanghai Children’s Hospital,School of Medicine,Shanghai Jiao Tong University,Shanghai 200062,China;Institute of Traditional Chinese Medicine,Tianjin University of Traditional Chinese Medicine,Tianjin 301617,China;Tianjin Key Laboratory of Therapeutic Substance of Traditional Chinese Medicine,Tianjin 301617,China)
出处
《药学实践与服务》
2025年第8期390-394,共5页
Journal of Pharmaceutical Practice and Service
基金
上海交通大学医学院高水平地方高校建设项目(二期)(2022zxy008)
上海市药学会上海青年药学人才能力提升项目(沪药学会字[2023]04号)。
