固相萃取辅助UPLC-MS/MS同时测定肾康宁胶囊中乌头类生物碱的含量  

Simultaneous determination of eight aconitum alkaloids in Shenkangning capsules by UPLC-MS/MS assisted by solid phase extraction

作　　者：刘世欣 陈良妮 程雪梅 季莉莉 李小锋 刘胜 康兴东 尉小慧 王长虹 LIU Shi-xin;CHEN Liang-ni;CHENG Xue-mei;JI Li-li;LI Xiao-feng;LIU Sheng;KANG Xing-dong;WEI Xiao-hui;WANG Chang-hong(Institute of Chinese Materia Medica,Shanghai Key Laboratory of Compound Chinese Medicines,The MOE Key Laboratory for Standardization of Chinese Medicines,Shanghai University of Traditional Chinese Medicine,Shanghai 201203,China;Jiangxi Puzheng Pharmaceutical Co.,Ltd.,Ji'an 331409,China)

机构地区：[1]上海中医药大学中药研究所,上海市复方中药重点实验室,中药标准化教育部重点实验室,上海201203 [2]江西普正制药股份有限公司,吉安331409

出　　处：《药物分析杂志》2022年第2期302-311,共10页Chinese Journal of Pharmaceutical Analysis

基　　金：国家重点研发计划(2018YFC1707302;2018YFC1707303)资助。

摘　　要：目的:建立肾康宁胶囊中乌头类生物碱的含量测定方法。方法:采用Waters ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm),以0.1%甲酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速0.3 mL·min^(-1),柱温40℃;质谱采用电喷雾离子化源(ESI),正离子模式下选择多反应监测(MRM)模式检测,建立同时测定肾康宁胶囊中乌头碱、新乌头碱、次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱、乌头原碱和新乌头原碱8个生物碱含量的固相萃取(SPE)辅助UPLC-MS/MS分析方法。结果:乌头碱、新乌头碱、次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱、乌头原碱、新乌头原碱分别在0.31~99.80、0.78~99.80、0.31~75.15、30.31~485.00、309.38~3712.50、61.88~742.50、7.75~248.00、61.25~1960.00 ng·mL^(-1)的质量浓度范围内线性关系良好,精密度、重复性和稳定性的RSD均小于5%,加样回收率在80.6%~109.0%之间。12批胶囊中次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱、乌头原碱和新乌头原碱含量范围分别为0.002~0.041、1.163~1.758、9.300~16.446、2.070~3.112、0.166~0.319、1.243~3.067μg·粒^(-1)。结论:建立的方法稳定可靠,可用于肾康宁胶囊的质量控制。Objective:To establish a method for determination of aconitine alkaloids in Shenkangning capsules.Methods:The determination was performed on a Waters ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8μm).The mobile phase was consisted of 0.1%formic acid solution(A)-acetonitrile(B)in gradient elution,the flow rate was 0.3 mL·min^(-1)and the column temperature was 40℃.The analytes were determined by electrospray ionization source(ESI)combined with multiple reaction monitoring(MRM)in positive ion mode.To establish a SPE-UPLC-MS/MS method for the determination of aconitine,hypaconitine,mesaconitine,benzoylaconine,benzoylhypaconine,benzoylmesaconine,aconine and mesaconine in Shenkangning capsules.Results:Aconitine,hypaconitine,mesaconitine,benzoylaconine,benzoylhypaconine,benzoylmesaconine,aconine and mesaconine showed good linearities in the ranges of 0.31-99.80,0.78-99.80,0.31-75.15,30.31-485.00,309.38-3712.50,61.88-742.50,7.75-248.00,and 61.25-1960.00 ng·mL^(-1),respectively.The RSDs of the precision,repeatability and stability tests were below 5%.The average recoveries were in the range of 80.6%-109.0%.The contents of mesaconitine,benzoylaconine,benzoylhypaconine,benzoylmesaconine,aconine and mesaconine in 12 batches of Shenkangning capsules were 0.002-0.041,1.163-1.758,9.300-16.446,2.070-3.112,0.166-0.319,and 1.243-3.067μg per capsule,respectively.Conclusion:The method is stable and reliable,and can be used for quality control of Shenkangning capsules.

关 键 词：肾康宁胶囊 乌头类生物碱 固相萃取 超高效液相色谱串联质谱 含量测定 

分 类 号：R917[医药卫生—药物分析学]