HPLC-MS/MS测定氯羟吡啶在牛奶中的残留

Determination of clopidol in milk by HPLC-MS/MS

建立了牛奶中氯羟吡啶残留检测的高效液相色谱-串联质谱方法（HPLC-MS/MS）。样品经乙腈提取,碱性氧化铝固相萃取柱（Alumina-B）净化,以乙腈＋0.1%甲酸水溶液作为流动相洗脱,采用电喷雾离子源（ESI）,多反应监测（MRM）方式进行采集,外标法定量。结果表明,氯羟吡啶在1-200ng·m L^-1浓度范围内呈现良好的线性关系,相关系数R2大于0.99,方法检测限为0.2μg·kg^-1,从5、10和50μg·kg^-13个水平添加浓度检测结果可以看出,方法回收率在93.4%-102.6%,相对标准偏差不大于6.5%。

A high performance liquid chromatography-mass / mass（ HPLC-MS / MS） method was established for the determination of clopidol in milk. The clopidol was extracted by acetonitrile,purified by Alumina-B. Analyzed with a methanol-0. 1% formic acid solution-acetonitrile mobile phase. The residues of clopidol were determined by electrospray ionization-trandem mass spectrometry,and quantified by the method of external standard. The calibration curve was good linear between the ratio of the peak areas and the concentrations of from 1 to 200 ng·m L^-1,the correlation coefficient R^2〉0. 99. The limit of detection of the method was 0. 2μg·kg^-1. The average recoveries from spiked at the three concentrations of 5,10 and 50 μg·kg^-1,ranged from93. 4% - 102. 6%,the relative standard results was not more than 6. 5%.