摘要
目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)同时检测五倍子洗剂中没食子酸、紫丁香苷、黄柏碱、秦皮乙素、大黄酸的含量。方法采用UPLC-MS/MS法,色谱柱为Agilent Poroshell 120 EC-C18(2.1 mm×150 mm,2.7μm),流动相为0.2%甲酸溶液-乙腈,梯度洗脱,流速为0.3 ml/min,柱温30℃;进样量2μl。质谱检测采用动态多反应离子检测模式(DMRM)。结果没食子酸、紫丁香苷、黄柏碱、秦皮乙素、大黄酸分别在153.8~15380、10.31~1031、5.265~526.5、50.70~5070、1.054~105.4 ng/ml浓度范围内线性关系良好,其精密度、重复性、稳定性和加样回收率均良好。结论该UPLC-MS/MS法稳定、快速、重复性好,适用于检测五倍子洗剂中没食子酸、紫丁香苷、黄柏碱、秦皮乙素、大黄酸的含量。
Objective To develop an ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method to simultaneously detect the contents of gallic acid,syringin,phellodendrine,aesculin and rhein in the gallnut lotion.Methods An UPLC-MS/MS method was established.Separation was performed on an Agilent Poroshell 120 EC-C18(2.1 mm×150 mm,2.7μm)with a gradient mobile phase system of 0.2%formic water-acetonitrile solution.The flow rate was 0.3 ml/min.The temperature of column was 30℃.The injection volume was 2μl.The MS detection was in dynamic MRM mode.Results gallic acid,syringin,phellodendrine,aesculin and rhein were successfully separated using this method,with good linear relationship as the ranges of 153.8-15380、10.31-1031、5.265-526.5、50.70-5070、1.054-105.4 ng/ml,respectively.The precision,repeatability,stability and recovery were good.Conclusion This UPLC-MS/MS method is stable,rapid,and reproducible.,It is suitable for detecting the contents of gallic acid,syringin,phellodendrine,esculetin and in the gallnut lotion.
作者
张群
陈瑜
支晓伟
须秋萍
杨英楠
赵亮
李盛建
ZHANG Qun;CHEN Yu;ZHI Xiaowei;XU Qiuping;YANG Yingnan;ZHAO Liang;LI Chengjian(Shanghai Baoshan Aged-nursing Hospital,Shanghai 200431,China;Luodian Hospital of Baoshan District,Shanghai 201908,China)
出处
《药学实践杂志》
CAS
2021年第5期437-441,共5页
Journal of Pharmaceutical Practice
基金
宝山区医学特色专科和社区项目建设课题(BSZK-2018-A10,BSZK-2019-C03)
宝山区罗店医院科研课题(20-A-6)。