摘要
依据国标GB 31658.17-2021《动物性食品中四环素类、磺胺类和喹诺酮类药物残留量的测定液相色谱-串联质谱法》,对鸡肉中10种喹诺酮药物残留量测定进行了不确定度评定.通过对该方法检测步骤的全面分析建立了不确定度数学模型,详细分析了主要包括喹诺酮类药物标准品配制、校准曲线制作、样品前处理、重复性试验、加标回收试验、仪器设备检测同时计算出该方法合成相对标准不确定度及相对扩展不确定度.评定结果表明:当鸡肉中恩诺沙星、诺氟沙星、沙拉沙星、环丙沙星、氧氟沙星、洛美沙星、丹诺沙星、培氟沙星、氟甲喹、依诺沙星的残留量分别为 95.145、96.522、92.240、93.068、88.82、93.995、93.358、92.185、94.197、93.872 μg/kg 时,其扩展不确定度分别为7.650、5.270、6.863、7.183、7.727、6.222、8.981、7.209、7.760、6.947 µg/kg(k=2,置信概率为 P=95％).该试验研究为鸡肉中10种喹诺酮类药物残留检测方法验证和检测结果的准确性判定提供了数据分析依据.
Abstract
According to the national standard GB 31658.17-2021＜Determination of tetracyclines,sulfonamides and determination of quinolones residual quantity in food of animal origin by HPLC-MS/MS＞,the uncertainties of 10 fluoroquinolones residues in chicken was evaluated.Through the comprehensive analysis of the detection steps of this method,the corresponding mathematical model was established,and the uncertainty components introduced mainly including the preparation of fluoroquinolones standard solution,standard curve fitting,sample pretreatment process,measurement repeatability,method spiking recovery rate,instrument measurement,etc.were analyzed in detail.At the same time,the synthesized comparative criterion indeterminacy and the patulous comparative criterion indeterminacy were computed.The results showed that the residues of enrofloxacin,norfloxacin,salafloxacin,ciprofloxacin,ofloxacin,lomefloxacin,danofloxacin,pefloxacin,fluoroquine and enoxacin in chicken were 95.145,96.522,92.240,93.068,88.82,93.995,93.358,92.185,94.197,93.872 μg/kg,respectively,the expanded uncertainty were 7.650,5.270,6.863,7.183,7.727,6.222,8.981,7.209,7.760,6.947 μg/kg,respectively(k=2,confidence probability P=95％).The evaluation results provide a reference for the objective evaluation of the accuracy of the detection results of 10 fluoroquinolones in animal derived food,and provide a data analysis basis for the validation of the detection methods of fluoroquinolones in chicken and the accuracy determination of the detection results.
基金项目
甘肃省农产品质量监管项目经费文件(甘农财发[2022]9号)
NETL
NSTL
万方数据