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评定
Uncertainty evaluation for determination of cyromazine in animal foods by high-performance liquid chromatography
王洁鑫 1王凤香 1张萌 1王瑞冬 1东诗迪 1刘佳 1陈修红1
作者信息
- 1. 国家副食品质量检验检测中心,国贸食品科学研究院有限公司,北京 102209;营养健康与食品安全北京市重点实验室,中粮营养健康研究院有限公司,北京 102209
- 折叠
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 19.8 μg/kg,扩展不确定度为 3.2 μg/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.
Abstract
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 19.8 μg/kg,with an expanded uncertainty of 3.2 μg/kg.Conclusion The main factors affecting uncertainty are the determination of standard,samples,the preparation of standard curves and the fitting of standard curves.
关键词
动物性食品/环丙氨嗪/高效液相色谱法/不确定度Key words
animal foods/cyromazine/highperformance liquid chromatography/uncertainty引用本文复制引用
出版年
2024
NETL
NSTL
万方数据