摘要
目的:建立UPLC-MS/MS法快速测定风湿马钱片、风湿安泰片、风湿骨康片和舒筋丸中马钱子碱与士的宁的含量。方法:色谱柱为Agilent Zorbax Eclipse Plus C18(2.1 mm×100 mm,1.8μm),以0.1%甲酸铵溶液-甲醇(75∶25,用甲酸调节pH至3.0)为流动相,流速为0.2 mL·min-1,柱温为35℃,进样量为1μL;采用电喷雾离子源(ESI)在正离子模式下,利用多反应监测(MRM)模式对马钱子碱和士的宁进行定量分析。结果:马钱子碱在2.6037~41.6590μg·mL-1线性关系良好,平均回收率为99.3%(n=9,RSD=1.9%)、士的宁在5.2923~84.6771μg·mL-1范围内线性关系良好,平均回收率为99.5%(n=9,RSD=1.1%)。结论:本方法快速、灵敏度高、准确可靠,适合多种抗风湿类中成药中马钱子碱与士的宁的定量分析。
OBJECTIVE To develop a LC-MS/MS method for the determination of strychnine and brucine in Fengshimaqian tablets,Fengshi Antai tablets,Fengshi Gukang tablets and Shujin pills.METHODS The analytical column was packed with Agilent Zorbax Eclipse Plus C18(2.1 mm×100 mm,1.8μm).The mobile phase was 0.1%ammonium formate solution-methanol(75:25,pH adjusted to 3.0 with formic acid)at a flow rate of 0.2 mL·min-1,the column temperature was 35℃and the injection volume was 1μL with electrospray positive ionization(ESI+).Multiple reaction monitoring(MRM)mode was used to detect strychnine and brucine.RESULTS The linear range of strychnine was 2.6037-41.6590μg·mL-1,and the brucine was 5.2923-84.6771μg·mL-1.The average recovery rate of strychnine was 99.3%(n=9,RSD=1.9%),and the average recovery rate of brucine was 99.5%(n=9,RSD=1.1%).CONCLUSION The method is rapid,sensitive,accurate,reliable and simple.It is suitable for quantitative analysis of strychnine and strychnine in various anti-rheumatic Chinese patent medicines.
作者
韦立志
李发娟
巫丽丽
WEI Li-zhi;LI Fa-juan;WU Li-li(The second affiliated hospital of Guangxi Medical university,Guangxi Nanning530007,China;The affiliated Tumor Hospital Of Guangxi Medical University,Guangxi Nanning 530021,China)
出处
《中国医院药学杂志》
CAS
北大核心
2020年第2期178-183,共6页
Chinese Journal of Hospital Pharmacy