摘要
目的:评估使用超高效液相色谱质谱联用仪测定水产品中孔雀石绿和结晶紫残留量过程的测量不确定度。方法:基于国家标准方法 GB/T19857-2005《水产品中孔雀石绿和结晶紫残留量的测定》原理,利用超高效液相色谱质谱联用仪对水产品中孔雀石绿和结晶紫残留量进行检测,通过对测定方法中的关键环节进行分析,建立测量不确定度评估模型,并计算合成测量不确定度。结果:在本试验条件下,选择95%置信概率,孔雀石绿含量测量结果应表示为(9.976±1.85)μg·kg^(-1)、隐色孔雀石绿为(10.186±1.550)μg·kg^(-1)、结晶紫含量为(9.482±0.902)μg·kg^(-1)、隐色结晶紫为(10.148±0.796)μg·kg^(-1)。结论:测量不确定度主要来源于样品提取液浓度测定,而加标回收、样品定容体积、重现性、称取样品质量对测量不确定贡献相对较小。
Objective:Evaluation of uncertainty in determination of malachite green and crystal violet residues in aquatic products by ultra-high performance liquid chromatography-mass spectrometry.Methods:Based on the principle of GB/T 19857-2005,the residues of malachite green and crystal violet in aquatic products were detected by ultra-high performance liquid chromatography-mass spectrometry(UHPLCMS).Through the analysis of key links in the determination method,the evaluation model of measurement uncertainty was established and the uncertainty of synthetic measurement was calculated.Results:Under the condition of this experiment,with 95%confidence probability,the measurement results of malachite green content should be expressed as(9.976+1.85)μg·kg^-1,leucomalachite green(10.186+1.550)μg·kg^-1,crystal violet(9.482+0.902)μg·kg-1,leucocrystal violet(10.148+0.796)μg·kg^-1.Conclusion:The uncertainty of measurement is mainly derived from the determination of the concentration of sample extract,while the contribution of standard recovery,constant volume,reproducibility and weighing sample quality to the uncertainty of measurement is relatively small.
作者
肖聪伟
Xiao Congwei(Jiangxi Institute for Food Control,Nanchang 330001,China)
出处
《现代食品》
2018年第22期108-115,共8页
Modern Food
