液相色谱-串联质谱法测定草鱼中磺胺类药物的不确定度评定

Evaluation of uncertainty in the determination of sulfonamides in grass carp by liquid chromatography tandem mass spectrometry

对液相色谱—串联质谱法测定水产品中磺胺类药物残留量的测量不确定度进行评定,建立草鱼(Ctenopharyngodon idella)中10种磺胺类残留量测定的不确定度评估数学模型。通过对测量不确定度的分量来源进行分析,计算各分量的不确定度与合成不确定度。结果表明,影响测定结果不确定度的主要因素为标准溶液的配制和标准曲线拟合,其次是测量重复性。在实际操作过程中,应尽量提高实验人员的操作规范性,并选择经过检定校准的玻璃器具,提高标准曲线的线性系数,严格管理和维护仪器设备,保持稳定性,保证检测结果的准确度,降低测量结果的不确定度。

In this study,the evaluation of uncertainty in the determination of sulfonamides residues in aquatic products by liquid chromatography tandem mass spectrometry was performed,and the uncertainty evaluation mathematical model of the determination of 10 sulfonamides residues in grass carp(Ctenopharyngodon idella)was established.The uncertainty of each component and combined uncertainty were calculated through analysis for component sources of measurement uncertainty.The results showed that the main factors affecting the uncertainty of determination results were standard solution preparation and standard curve fitting,followed by measurement repeatability.In the actual operation process,the operating specifications of the experimental personnel should be improved as far as possible,and the calibrated glass wares should be selected.Meanwhile,the linear coefficient of the standard curve should be improved and the equipment should be strictly managed and maintained to keep stability,ensure the accuracy of determination results and reduce the uncertainty of measurement results.