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《化学分析计量》 2022年第06期
DOI:10.3969/j.issn.1008-6145.2022.06.020
柱后衍生-液相色谱法测定蔬菜中克百威残留量的不确定度
黄小清,王宇,刘佳,谭锦萍,林泽珊,王成龙,黄松,赵金利
广州市食品检验所,广州 511400 
Evaluation of uncertainty for determination of carbofuran residues in vegetablesby liquid chromatography with post-column derivatization
HUANG Xiaoqing, WANG Yu, LIU Jia, TAN Jinping,
LIN Zeshan, WANG Chenglong, HUANG Song, ZHAO Jinli(Guangzhou Institute for Food Inspection, Guangzhou 511400, China) 
摘要:评定柱后衍生-液相色谱法测定蔬菜中克百威残留量的不确定度。根据JJF 1059.1—2012《测量不确定度评定与表示》和JJF 1135—2005《化学分析测量不确定度评定》中有关规定,对该方法建立不确定度评估结果计算的数学模型,对测定中的不确定度来源进行分析和评估。测量不确定度的主要来源包括标准溶液稀释过程、样品的称量、样品溶液的稀释定容、重复性测量,分别对不确定度分量进行计算,并合成相对标准不确定度。当蔬菜中克百威和3-羟基克百威残留量为0.020 mg/kg时,扩展不确定度分别为0.001 3、0.001 6 mg/kg(k=2),克百威和3-羟基克百威残留量分别表示为(0.020±0.001 3)、(0.020±0.001 6) mg/kg(k=2)。该方法确定了不确定度主要来源为标准溶液的稀释过程,为检验结果的准确性及可靠性提供了技术依据。 
Abstract:A method for evaluating the uncertainty of determination of carbofuran residues in vegetables by post column derivatization liquid chromatography was established. According to JJF 1059.1—2012 Evaluation and Expression of Uncertainty in Measurement and JJF 1135—2005 Evaluation of Uncertainty in Chemical Analysis Measurement, a mathematical model of uncertainty evaluation results was established for the developed method, and the sources of uncertainty in measurement were analyzed and evaluated. The main sources of measurement uncertainty include the dilution process of standard solution, sample weighing, dilution and constant volume of sample solution, and repeatability measurement. The uncertainty components were calculated respectively, and the relative standard uncertainty was synthesized. The uncertainty components were respectively calculated, and the relative standard uncertainty was synthesized. The expanded uncertainty was 0.001 3 mg/kg and 0.001 6 mg/kg(k=2), respectively, when the residues of carbofuran and 3-hydroxycarbofuran in vegetables were 0.02 mg/kg. The residues of carbofuran and 3-hydroxycarbofuran might be expressed as (0.020±0.001 3) mg/kg(k=2) and (0.020±0.001 6) mg/kg(k=2), respectively. This method determines that the main source of uncertainty is the dilution process of standard solution, which provides a technical basis for the accuracy and reliability of test results. 
关键词:克百威;3-羟基克百威;蔬菜;不确定度;液相色谱法;柱后衍生法 
Keywords:carbofuran; 3-hydroxycarbofuran; vegetables; uncertainty; liquid chromatography; post-columnderivatization 
基金:广州市市场监督管理局科技项目(2021kj51) 
本文引用格式:
黄小清,王宇,刘佳,等.柱后衍生-液相色谱法测定蔬菜中克百威残留量的不确定度[J].化学分析计量,2022,31(6):87.
HUANG Xiaoqing,WANG Yu,LIU Jia,et al. Evaluation of uncertainty for determination of carbofuran residues in vegetables by liquid chromatography with post-column derivatization[J]. Chemical Analysis and Meterage,2022,31(6):87. 

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