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《化学分析计量》 2020年第03期
DOI:10.3969/j.issn.1008-6145.2020.03.023
鸡蛋中氟虫腈砜能力验证样品单元内与单元间均匀性评价案例与模型分析
张会亮,程琳,高晓明,项新华,王海燕,孙磊,王聪
中国食品药品检定研究院,北京 100050 
Case and model analysis of between-unit and within-unit homogeneity evaluation for the proficiency test sample of fipronil sulfone in eggs
张会亮,程琳,高晓明,项新华,王海燕,孙磊,王聪
National Institutes for Food and Drug Control, Beijing 100050, China 
摘要:对鸡蛋中氟虫腈砜能力验证样品进行单元内均匀性和单元间均匀性评价。对能力验证涉及的检测方法进行方法学考察,按照预设的模型,在单元内和单元间取样检测。使用单元内子样结果均方差和方法重复性均方差构建单因素方差分析模型,完成了单元内均匀性评价。对单元间和单元内均匀性评价的方差分析模型中组间和组内方差的来源及代表性进行了讨论。结果表明鸡蛋中氟虫腈砜样品的单元内均匀性和单元间均匀性满足要求。开展单元内均匀性评价有利于掌握能力验证方法性能,确认检测最小取样量,识别不均匀性来源,增加单元间均匀性评价的可靠性。建立的单元内均匀性评价模型克服了标准模型中多次转化测量数据难以获得的问题,可在各类能力验证项目中推广应用。 
Abstract:The within-unit and between-unit homogeneity evaluation of proficiency test sample of fipronil sulfone in eggs was conducted. The detection method involved in the proficiency test was investigated in methodology, and samples were taken within and between units for detection according to the pre-set model. Within-unit homogeneity evaluation was conducted with one-way ANOVA (Analysis of variance) model by using the variance of intra unit test data and variance of method repeatability data. The results showed that the within-unit and between-unit homogeneity of fipronil sulfone meet the requirements. The sources and representativeness of variance in the one-way ANOVA model of between-unit and within-unit homogeneity evaluation was discussed. A within-unit homogeneity evaluation is conducive to mastering the performance of the method involved in proficiency test, confirming the minimum sampling amount of the measurement, identifying the source of the inhomogeneity, and increasing the reliability of the between-unit homogeneity evaluation. The within-unit homogeneity evaluation model established can overcome the problem in obtaining the multi transformation data in the standard model, and can be widely used in various capacity verification projects. 
关键词:能力验证;均匀性评价;方差分析;单元内;单元间 
Keywords:proficiency test; homogeneity evaluation; variance analysis; within-unit; between-unit 
基金:“十三五”国家重点研发计划重点专项(2017YFC1601300) 
本文引用格式:
张会亮,程琳,高晓明,等.鸡蛋中氟虫腈砜能力验证样品单元内与单元间均匀性评价案例与模型分析[J].化学分析计量,2020,29(3):101-106.
ZHANG H L,CHENG L,GAO X M,et al. Case and model analysis of between-unit and within-unit homogeneity evaluation of the proficiency test sample of fipronil sulfone in eggs[J]. Chemical analysis and meterage,2020,29(3):101-106. 

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