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目的:建立LC-MS/MS测定大鼠血浆中的马钱子碱和士的宁含量,以溶剂萃取法提取大鼠血浆中的待测成分。方法:以他克林为内标,采用Agilent ZORBAX XDB-C18色谱柱,流动相为乙腈-甲醇-水(0.05%甲酸,10 nmol.L-1甲酸铵)梯度洗脱,质谱采用多反应监测(MRM),用于定量分析的离子对依次为m/z 395.2/324.2(马钱子碱),m/z 335.2/184.2(士的宁)和m/z 199.1/171.1(他克林)。结果:测定血浆样品2种成分的线性范围分别为0.195～100,0.078 1～40μg.L-1,相关系数分别为0.994,0.996,马钱子碱的提取回收率为78.9%～102.4%,士的宁的提取回收率为95.2%～106.1%,方法的精密度、准确度、基质效应和稳定性均符合要求。结论:方法专属性强、灵敏度高,适用于血浆马钱子类生物碱的药代动力学研究。囊泡制剂能够降低马钱子碱进入体循环的药物浓度,且具有缓释作用。
OBJECTIVE: To establish a method for the determination of brucine and strychnine in rat plasma by LC-MS / MS, and to extract the analytes from rat plasma by solvent extraction. Methods: Tacrin was used as internal standard. The mobile phase was acetonitrile-methanol-water (0.05% formic acid, 10 nmol.L-1 ammonium formate) gradient on an Agilent ZORBAX XDB-C18 column. MS was monitored by multiple reaction monitoring (MRM) and ion pairs for quantitative analysis were m / z 395.2 / 324.2 (strychnine), m / z 335.2 / 184.2 (strychnine) and m / z 199.1 / 171.1 (tacrine) in turn. Results: The linear range of the two components in the plasma samples were 0.195-100 and 0.078 1-40 μg.L-1 respectively, the correlation coefficients were 0.994 and 0.996 respectively, the recoveries of brucine were 78.9% -102.4% The extraction recovery of Ning was 95.2% -106.1%. The precision, accuracy, matrix effect and stability of the method met the requirements. Conclusion: The method is specific, sensitive and suitable for the pharmacokinetic study of plasma Strychnos alkaloids. Vesicle preparations can reduce the drug concentration of brucine into the systemic circulation and have a sustained release effect.