高效液相色谱-串联质谱法测定猪肉中可的松和氢化可的松残留量的不确定度评价

Uncertainty Evaluation for the Detection of Cortisone and Hydrocortisone Residues in Pork by High Performance Liquid Chromatography-tandem Mass Spectrometry

关键词:  可的松  氢化可的松  不确定度评定

Key words:  Cortisone  Hydrocortisone  uncertainty evaluation

摘要:

评定超高效液相色谱-串联质谱法测定猪肉中可的松和氢化可的松残留量的不确定度。以本单位自建方法XCZY-051《动物源食品中克仑特罗等51种兴奋剂的检测方法液相色谱-串联质谱法》为基础，结合CNAS-GL006《化学分析中的不确定度评估指南》，建立数学模型，以猪肉中检出率最高的内源性兴奋剂可的松和氢化可的松为例分析不确定度来源并计算各不确定度得到的合成标准不确定度。当样品中可的松含量为3.386 μg/kg时，其扩展不确定度为0.4374 μg/kg(k=2)；当氢化可的松含量为7.866 μg/kg时，其扩展不确定度为0.9690 μg/kg(k=2)。本方法的不确定度来源主要来自样品回收率、重复性、标准溶液配制和曲线拟合。

Abstract:

To evaluate the uncertainty for determination of cortisone and hydrocortisone residues in pork by ultra performance liquid chromatography-tandem mass spectrometry isotope internal standard method. Based on the self-developed method XCZY-051 Ultra liquid chromatography-tandem mass spectrometry for the detection of clenbuterol and other 51 stimulants in animal derived foods and according to CNAS-GL006 Guidance on evaluating the uncertainty in chemical analysis, a mathematical model was established, then take the endogenous stimulants cortisone and hydrocortisone with the highest detection rate in pork as examples, the source of uncertainty was analyzed and the synthetic standard uncertainty was calculated. When the cortisone residue in pork was 3.386 μg/kg, the expanded uncertainty was 0.4374 μg/kg(k=2). When the hydrocortisone residue in pork was 7.866 μg/kg, the expanded uncertainty was 0.9690 μg/kg(k=2). The uncertainty of measurement mainly come from sample recovery, repeatability, the preparation of standards and curve fitting.