摘要
为了控制检测结果准确性,以鸡蛋粉中氟虫腈砜残留分析标准物质[GBW(E)100779]为测试样,采用“自下而上”法对基于多功能净化柱(PAC柱)净化的同位素稀释液相色谱串联质谱(ID-LC-MS/MS)法进行测量不确定度评估。“鱼骨图”分析表明,不确定度分量主要来源有样品称样量、内标溶液添加体积、标准工作溶液浓度及其移取体积。内标溶液添加体积引入的不确定度最大,对检测结果不确定度的贡献率为68.59%;万分之一天平称量引入的不确定度可忽略不计。同位素内标的添加过程是ID-LC-MS/MS法检测的关键控制点,参考基准的合理选择和目标物的完全提取是准确测量的前提。进一步用LC-MS/MS法对参考物质、稀释剂和内标溶液的适用性进行了评估,并基于国家有证标准物质[GBW(E)100779]对提取方法进行了优化。研究结果有利于提升鸡蛋食品安全的检测质量和质控水平,为精准检测质控方案的设计提供新思路。
In order to control the accuracy of the detection results,the“Bottom-up”method and a national certified reference material[GBW(E)100779]were used to carry out the measurement uncertainty evaluation on the determination of fipronil-sulfone in egg powder by PAC cartridge-based cleanup and isotope dilution-liquid chromatography-tandem mass spectrometry(ID-LC-MS/MS).The“fish-bone”diagram analysis showed that the main sources of uncertainty components were the sample weighing amount,the volume of internal standard solution added,the concentration of standard working solution and the volume taken.The uncertainty introduced by the addition volume of the internal standard solution was the largest,contributing 68.59%to the uncertainty of the detection results.The uncertainty introduced by the microbalance weighing,which is one in ten thousand,can be neglected.The addition process of the isotope internal standard is a key control point for the ID-LC-MS/MS method,and the reasonable selection of the reference benchmark and the complete extraction of the target substance are prerequisites for accurate measurement.Furthermore,the applicability of the reference material,diluent solvent,and internal standard solution was evaluated using LC-MS/MS method,and the extraction method was optimized based on the national certified reference material[GBW(E)100779].The research results are beneficial to improving the detection quality and quality control level of egg food safety,and provide new ideas for the design of precise detection quality control schemes.
作者
张巧艳
方维焕
郑蔚然
王夏君
刘超纲
王强
ZHANG Qiaoyan;FANG Weihuan;ZHENG Weiran;WANG Xiajun;LIU Chaogang;WANG Qiang(Institute of Agro-Product Safety and Nutrition,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China;College of Animal Sciences,Zhejiang University,Hangzhou 310058,China;Institute of Crops and Nuclear Technology Utilization,Zhejiang Academy of Agricultural Sciences,Hangzhou 310021,China)
出处
《浙江农业学报》
CSCD
北大核心
2024年第3期643-650,共8页
Acta Agriculturae Zhejiangensis
基金
省部共建农产品质量安全危害因子与风险防控国家重点实验室开放基金(2010DS700124-KF2003)。
