UPLC-MS/MS快速测定4种抗风湿类中成药中马钱子碱与士的宁的含量

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，1.8 μm），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1 μL；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2.603 7~41.659 0 μg·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5.292 3~84.677 1 μg·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。

Rapid determination of strychnine and strychnine in 4 kinds of anti-rheumatic Chinese patent medicines by UPLC-MS/MS

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, 1.8 μm). 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 1 μL with electrospray positive ionization (ESI⁺). Multiple reaction monitoring (MRM) mode was used to detect strychnine and brucine. RESULTS The linear range of strychnine was 2.603 7-41.659 0 μg·mL^-1, and the brucine was 5.292 3-84.677 1 μg·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.