摘要
目的评定高效液相色谱法测定动物性食品中环丙氨嗪残留量的不确定度。方法样品经三氯乙酸和乙腈混合液多次均质提取,取上清液用正己烷除脂,再用水浴旋转蒸发浓缩,三氯乙酸和乙腈混合液复溶,再用混合阳离子交换固相萃取柱净化,经氨基色谱柱分离,以乙腈水作为流动相进行等度洗脱,二极管阵列检测器,外标法定量测定动物性食品中环丙氨嗪残留量。依据JJF 1135—2005《化学分析测量不确定度评定》和JJF 1059.1—2012《测量不确定度评定与表示》,评估整个检测过程中所产生的不确定度包含称量、标物、标准工作曲线配制、标准曲线拟合、样品测量重复性、仪器和加标回收率,并对各个因素引入的不确定度进行计算,最后得到扩展不确定度。结果当鸡肉中环丙氨嗪检测结果19.8μg/kg,扩展不确定度为3.2μg/kg。结论影响不确定度的主要因素是标准物质、样品的测量、标准曲线的配制和标准曲线的拟合。
Objective To evaluate of uncertainty in the determination of residual cyclopropamide in animal food by high-performance liquid chromatography.Methods The sample was repeatedly extracted by the mixture of Trichloroacetic acid and acetonitrile.The supernatant was degreased with n-hexane,and then concentrated by rotating evaporation in a water bath.The mixture of trichloroacetic acid and acetonitrile was redissolved,and then purified by a mixed cation exchange solid phase extraction column.After separation by an amino chromatographic column,acetonitrile water was used as the mobile phase for isocratic elution.The residue of cyclopromazine in animal food was quantitatively determined by diode array detector and external standard method.According to the JJF 1135-2005 Chemical Analysis Measurement Uncertainty Assessment and JJF 1059.1-2012 Measurement Uncertainty Assessment and Representation,the uncertaintygenerated during the entiretesting process includes weighing,standard,standard working curve formulation,standard curve fitting,sample measurement repeatability,instrument and standard recovery rate,and the uncertainty introduced by each factor is calculated,and finally theexpansionuncertainty is obtained.Results When the detection result of cyromazine in chicken was 19.8μg/kg,with an expanded uncertainty of 3.2μg/kg.Conclusion The main factors affecting uncertainty are the determination of standard,samples,the preparation of standard curves and the fitting of standard curves.
作者
王洁鑫
王凤香
张萌
王瑞冬
东诗迪
刘佳
陈修红
WANG Jie-Xin;WANG Feng-Xiang;ZHANG Meng;WANG Rui-Dong;DONG Shi-Di;LIU Jia;CHEN Xiu-Hong(National Non-Staple Food Quality Inspection and Testing Center,International Trade Food Science Research Institute Co.,Ltd.,Beijing 102209,China;Beijing Key Laboratory of Nutrition Health and Food Safety,Nutrition&Health Research Institute,COFCO Corporation,Beijing 102209,China)
出处
《实验室检测》
2024年第10期32-36,共5页
Laboratory Testing
关键词
动物性食品
环丙氨嗪
高效液相色谱法
不确定度
animal foods
cyromazine
highperformance liquid chromatography
uncertainty
