目的:建立了液相色谱-串联质谱法(LC-MS/MS)测定大鼠血浆中氯氨吡啶酸浓度的分析方法.方法:使用1％甲酸水调整血浆样本pH后,用含5％异丙醇的乙酸乙酯溶液萃取,萃取液浓缩后用流动相复溶后进行检测.LC-MS/MS方法采用Eclipse Plus C18色谱柱(2.1 mm×50 mm,1.8 μm),柱温40℃,流动相为甲醇和0.1％甲酸水,梯度洗脱,流速0.3 mL/min,电喷雾离子源正离子(ESI+),扫描离子模式:多反应监测(MRM),采用外标法定量.结果:氯氨吡啶酸在50.0～10 000 ng/mL范围内线性关系良好,相关系数＞0.99,选择性、准确度、精密度、基质效应、提取回收率和稳定性均满足接受标准的要求,建立的方法可用于氯氨吡啶酸大鼠毒代动力学研究.
The Analytical Method for the Detection of Aminopyralid in Rat Plasma was Validated using Liquid-mass Spectrometry
Objective:A liquid chromatography tandem mass spectrometry(LC-MS/MS)method is developed for the determi-nation of aminopyralid in rat plasma.Method:After adjusting the pH of the plasma sample with 1％formic acid,extraction with a solution of ethyl acetate containing 5％isopropanol.Concentrate the extraction and dissolve it in the mobile phase and then detect directly.The LC-MS/MS method is performed on Eclipse Plus C18 column(2.1 mm×50 mm,1.8 μm)at the temperature of4 0℃,by the gradient elution with methnol-0.1％formic acid as the mobile phase at the flow rate of 0.3 mU min.The positive electrospray ionization(ESI+)source under multiple reaction monitoring(MRM)mode and external stan-dard method are used for quantification.Results:The correlation coefficients up to 0.99 are obtained at the concentration rang of 50.0-10 000 ng/mL.The parameters of selectivity,accuracy,precision,matrix effect,recovery and stability are met the acceptance criteria.The method can be used for the toxicokinetic study of aminopyralid in rats.
liquid chromatography tandem mass spectrometryaminopyralid determinationtoxicokinetics
万方数据
维普
