液相色谱串联质谱法测定肉糜中克伦特罗 残留量的不确定度评定

Uncertainty evaluation for the determination of clenbuterol residues in meat by liquid chromatography tandem mass spectrometry

中文关键词:  液相色谱-质谱/质谱法  内标法  不确定度评定  克伦特罗

英文关键词:liquid chromatography tandem mass spectrometry  internal standard method  uncertainty evaluation  clenbuterol

中文摘要:

      目的 评定液相色谱-质谱/质谱法测定肉糜中克伦特罗残留量的不确定度。方法 根据JJF 1059.1-2012《测量不确定度评定与表示》, 考察称量、标准溶液的配制、样品提取净化、仪器测量等主要因素引入的不确定度, 并对不确定度的各分量进行计算和合成。结果 该方法测定肉糜中克伦特罗残留量的合成相对标准不确定度为0.0428, 肉糜中克伦特罗残留量测定结果为(18.8±1.6)μg/kg (P=95%, k=2)。结论 本实验的不确定度主要由标准溶液与内标物的峰面积比、样品与内标物的峰面积比、标准溶液和样品中内标物的浓度比引入。

英文摘要:

      Objective To evaluate the uncertainty of determination of clenbuterol in meat by liquid chromatography tandem mass spectrometry. Methods According to JJF 1059.1-2012 Measurement uncertainty evaluation and presentation, the uncertainty of main factors such as weighing, standard solution preparation, sample extraction and purification, apparatus measure were investigated, and the components of uncertainty were calculated and synthesized. Results The synthetic relative standard uncertainty of the method for the determination of clenbuterol residues in meat emulsion was 0.0428. The determination results of clenbuterol residues in mince meat was (18.8±1.6) μg/kg (P=95%, k=2). Conclusion The uncertainty of the method is mainly caused by peak area ratio of standard solution and internal standard, peak area ratio of sample and internal standard and concentration ratio of internal standard in standard solution and sample.