摘要
目的建立高效液相色谱-串联质谱(HPLC-MS/MS)法同时测定维康凝胶中6种乌头类生物碱(苯甲酰次乌头原碱、苯甲酰新乌头原碱、苯甲酰乌头原碱、次乌头碱、新乌头碱、乌头碱)及闹羊花毒素Ⅱ的含量。方法采用Agilent Infinitylab Poroshell 120 EC-C18色谱柱(4.6 mm×150 mm,4μm);以乙腈-0.1%甲酸水溶液为流动相,梯度洗脱;柱温30℃;流速0.45 mL/min;采用电喷雾离子源,正离子、多重反应监测模式检测。结果以空白基质配制对照品溶液,6种乌头类生物碱及闹羊花毒素Ⅱ在各自范围内线性关系良好(r≥0.9990),精密度、稳定性、重复性良好,平均加样回收率为81.56%~107.08%,相对标准偏差(RSD)为1.75%~4.78%。结论本研究所建含量测定方法克服了基质效应,灵敏度高、专属性强,可为维康凝胶实现“效-毒平衡”的质量控制策略提供实验基础。
Objective To establish an efficient high-performance liquid chromatography-tandem mass spectrometry(HPLCMS/MS)method for the simultaneous determination of six aconitine-type alkaloids(benzoylhypacoitine,benzoylmesaconine,benzoylaconine,hypaconitine,mesaconitine,aconitine)and rhodojaponinⅡin Weikang Gel.Methods Chromatographic separation was performed on an Agilent InfinityLab Poroshell 120 EC-C18 column(4.6 mm×150 mm,4μm)using acetonitrile-0.1%formic acid in water as the mobile phase with gradient elution;column temperature was 30°C and flow rate 0.45 mL/min.Detection was carried out by electrospray ionization in positive ion mode using multiple reaction monitoring.Results The reference solution was prepared with a blank matrix,and the linear relationship between the six aconitine alkaloids and rhodojaponinⅡwas good in their respective ranges(r≥0.9990).Precision,stability,and repeatability met method validation requirements.Mean spiked recoveries ranged from 81.56%to 107.08%,with relative standard deviations(RSDs)of 1.75%-4.78%.Conclusion The developed HPLC-MS/MS method overcomes matrix effects,offers high sensitivity and specificity,and can provide an experimental basis for quality control strategies aimed at balancing efficacy and toxicity of Weikang Gel.
作者
陈微微
李贤柳
刘延霞
林水兰
黄海福
张军
Chen Weiwei;Li Xianliu;Liu Yanxia;Lin Shuilan;Huang Haifu;Zhang Jun(School of Pharmaceutical Sciences,Guangzhou University of Chinese Medicine,Guangzhou 510006,China;Shenzhen TCM Oncology Medical Center,Shenzhen Guangdong 518000,China)
出处
《保健医学研究与实践》
2025年第9期25-33,共9页
Health Medicine Research and Practice
基金
国家自然科学基金项目(82374315)
深圳市“医疗卫生三名工程”项目(SZZYSM202311011)。
