摘要
目的 建立UPLC-MS/MS法同时测定风湿安泰片中单酯型生物碱(苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱)和双酯型生物碱(新乌头碱、次乌头碱、乌头碱)的含量,并对测定结果进行化学计量学分析及风险评价,为其质量控制提供依据。方法 采用Waters BEH C18色谱柱(2.1 mm×100 mm,1.7μm),以甲醇(A)-0.1%甲酸水溶液(B)为流动相,梯度洗脱,流速为0.3 mL·min-1,柱温35℃,进样量1μL;质谱采用电喷雾离子源(ESI),正离子检测,多反应监测(MRM)模式。结果 6个成分在各自范围内线性关系良好(r≥0.9990),平均加样回收率为90.3%-107.6%,RSD为0.9%-1.8%。23批样品中双酯型生物碱总量范围为1.35-19.49μg·片-1,安全性风险较低;单酯型生物碱总量范围为20.17-99.55μg·片~(-1);化学计量学结果显示,23批样品聚为4类,不同生产企业样品质量存在一定差异。结论 建立的方法稳定可靠,可用于风湿安泰片的质量控制。
Objective To establish a UPLC-MS/MS method to measure the content of monoester-alkaloids(benzoylmesaconine,benzoylaconine,benzoylhypaconine)and diester-alkaloids(mesaconitine,hyp-aconitine,aconitine)in Fengshiantai tablets.To provide a basis for quality control by conducting chemometric analysis and risk assessment on the measurement results.Methods The components were separated on Waters BEH C18 column(2.1 mm×100 mm,1.7μm)with methanol and 0.1%formicacid aqueous solution as the mobile phase by gradient elution at a flow rate of 0.3 mL·min^(-1).The column temperature was set at 35℃.The injection volume was 1μL.The detection was carried out by electrospray ionization(ESI),and electron spray ionization source was adopted in positiveion detection with multiple reaction monitoring mode(MRM).Results Six components showed good linear relationships within their own ranges(r≥0.9990),whose average recovery rate of samples were 90.3%-107.6%with the RSD of 0.9%-1.8%.In 23 batches of tested samples,the diester-alkaloids contents ranged from 1.35 to 19.49μg per tablet,which indicated low risk of drug safety;the monoester-alkaloids contents ranged from 20.17-99.55μg per tablet.The results of chemometrics showed that 23 batches of samples were classify into four categories,and there were certain differences in sample quality among different production enterprises.Conclusion The established method is stable and reliable,and can be used for quality control of Fengshi Antai tablets.
作者
张元元
王晓蕾
赵振霞
刘永利
孙慧珠
苏建
ZHANG Yuanyuan;WANG Xiaolei;ZHAO Zhenxia;LIU Yongli;SUN Huizhu;SU Jian(Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050227,China;The Pharmacovigilance Center of Hebei,Shijiazhuang 050000,China)
出处
《世界科学技术-中医药现代化》
CSCD
北大核心
2024年第8期2168-2174,共7页
Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology
基金
河北省药品监督管理局科技计划项目(2023ZC1018):风湿安泰片的质量控制方法研究
负责人:张元元。
