液相色谱-串联质谱法测定生鲜乳中氯噻嗪残留量  

Determination of Residue in Raw Milk by Liquid Chromatography-Electrospray Tandem Mass Spectrometry

作　　者：田素润[1] 蒋俊树[1] 丁磊[1] 

机构地区：[1]安徽国家农业标准化与监测中心,合肥230051

出　　处：《化学分析计量》2013年第3期17-19,共3页Chemical Analysis And Meterage

基　　金：国家质检总局科技计划项目(2012QK003)

摘　　要：采用液相色谱-串联质谱(HPLC-ESI-MS/MS)法测定生鲜乳中氯噻嗪含量。样品经去脂净化后,用乙酸乙酯提取,采用液相色谱-串联质谱法分析,多反应监测模式下(MRM)外标法定量。结果表明氯噻嗪的质量浓度与定量离子的峰面积在5～100μg/L范围内线性良好,线性相关系数为r=0.999,定量限为5μg/kg(S/N=10),在0.01,0.05,0.1 mg/kg的添加水平下,回收率在86%～105%之间,测定结果的相对标准偏差小于8%(n=6)。该方法前处理过程简便快捷,可满足实验室大量、快速分析的需求。A new method of ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry （LC-ESI-MS /MS） for the analysis of chlorothiazide in raw milk was developed. After degreasing purification, the sample was extracted by ethyl acetate, and then chlorothiazide in which was determined by LC-ESI-MS/MS. Separated analytes were determined using multiple reaction monitoring （MRM）. The quantitative analysis of target compounds was performed by the external standard method. The result indicated that the calibration curves were linear in the range of 5-100 μg/L for chlorothiazide. The correlation coefficients was 0.999. The quantification limit was 5 μg/L （S/N=1 0）. The recoveries of chlorothiazide at three spiked levels of 0.01,0.05,0.1 mg/kg were in the range of 86%-105% with RSDs （n=6） less than 8%. This method shortened the time ofpre-treatment process, and the result was credible. It could satisfy the requirement of mass and fast analysis in the laboratory.

关 键 词：生鲜乳 氯噻嗪 液相色谱串联质谱 测定 

分 类 号：O657.7[理学—分析化学]