固相萃取-高效液相色谱-串联质谱法检测动物组织和水产品中曲美他嗪含量

Determination of trimetazidine content in animal tissues and aquatic products by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry

建立通过固相萃取-高效液相色谱-串联质谱法测定动物组织和水产品中曲美他嗪的方法。样品经体积分数0.2%甲酸乙腈溶液涡旋超声提取,再经混合型强阳离子交换固相萃取柱Cleanert PCX净化,用3 mL体积分数3%氨水甲醇洗脱,净化液浓缩后用1 mL初始流动相(乙腈与体积分数0.1%甲酸水体积比2∶8)复溶,经尼龙膜过滤上机检测;建立的方法采用InertSustain C18色谱柱、电喷雾正离子模式(ESI+)和多反应离子监测模式(MRM)检测,基质匹配内标法定量。结果表明:在动物组织和水产品基质中,曲美他嗪在0.3~10 ng/mL质量浓度范围内线性关系良好,决定系数均≥0.998,平均回收率为92.3%~109.6%,相对标准偏差为3.9%~12.5%。建立的方法可满足目标物检测的准确度、精密度和灵敏度要求。

A method for the determination of trimetazidine in animal tissues and aquatic products by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry was established.The samples were extracted by vortex ultrasound with volume fraction 0.2%formic acid acetonitrile solution,purified by mixed strong cation exchange solid-phase extraction column Cleanert PCX,eluted with 3 mL volume fraction 3%ammonia water methanol solution,and then redissolved with 1 mL initial mobile phase after concentration(volume ratio of acetonitrile to volume fraction 0.1%formic acid water 2∶8).The sample was then filtered and tested on the NYLON membrane.The method was established by Intertsustain C_(18)reversed-phase column,electrospray positive ion mode(ESI~+)and multi reaction ion monitoring mode(MRM)for detection,and the matrix matching internal standard method for quantification.The results showed that in the matrice of animal tissues and aquatic product matrices,trimetazidine had a good linear relationship within the mass concentration of 0.3-10 ng/mL,with determination coefficients≥0.998,average recovery rates from 92.3%to 109.6%,and relative standard deviation from 3.9%to 12.5%.The method could meet the accuracy,precision,and sensitivity requirements for target object detection.