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实验室在测定脆饼干中丙烯酰胺方面的性能评估。

Assessment of performance of laboratories in determining acrylamide in crispbread.

作者信息

Clarke Don B, Kelly Janet, Wilson Lesley A

机构信息

Department for Environment Food and Rural Affairs, Central Science Laboratory, Sand Hutton, York, United Kingdom.

出版信息

J AOAC Int. 2002 Nov-Dec;85(6):1370-3.

Abstract

A proficiency testing round was undertaken to assess the performance of laboratories to measure acrylamide in a sample of crispbread. Retail samples of crispbread were ground to a fine powder and after thorough mixing were packed in 40 g units for distribution. Ten samples were selected at random and analyzed in duplicate for acrylamide by liquid chromatography/mass spectrometry (LC/MS). Standard statistical tests showed that the material was homogeneous for the purposes of proficiency testing. Test samples were distributed to 55 laboratories in 16 countries in Europe, North America, Australia, and the Middle East. The results were analyzed by standard proficiency testing statistical procedures, and laboratories were awarded z-scores on the basis of their reported results. Based on a target standard deviation (sigmap value) taken from the Horwitz equation, for a robust mean value of 1.2 mg/kg acrylamide, satisfactory results (z-score within +/- 2 for those between 0.8 and 1.6 mg/kg) were obtained by 86% of the 37 laboratories that returned results. Only 1 laboratory was unsatisfactory and 4 had questionable results. About equal numbers of laboratories used gas chromatography (GC)/MS and LC/MS procedures with about 25% using MS/MS and one using GC with electron capture detection. There was no evident trend in performance or bias in results. GC/MS and LC/MS data were evenly distributed across the population of laboratories reporting results.

摘要

开展了一轮能力验证测试,以评估各实验室测定脆饼干样品中丙烯酰胺含量的表现。将零售的脆饼干样品研磨成细粉,充分混合后以40克的单位进行包装以便分发。随机选取10个样品,采用液相色谱/质谱联用仪(LC/MS)对丙烯酰胺进行一式两份分析。标准统计测试表明,就能力验证测试而言,该材料是均匀的。测试样品分发给了欧洲、北美、澳大利亚和中东16个国家的55个实验室。结果通过标准能力验证测试统计程序进行分析,并根据各实验室报告的结果为其赋予z分数。根据取自霍维茨方程的目标标准偏差(sigmap值),对于丙烯酰胺的稳健平均值为1.2毫克/千克,返回结果的37个实验室中有86%获得了满意结果(对于0.8至1.6毫克/千克之间的结果,z分数在+/-2以内)。只有1个实验室结果不满意,4个实验室结果存疑。使用气相色谱(GC)/MS和LC/MS程序的实验室数量大致相同,约25%的实验室使用串联质谱(MS/MS),1个实验室使用带电子捕获检测的气相色谱。在性能或结果偏差方面没有明显趋势。GC/MS和LC/MS数据在报告结果的实验室群体中均匀分布。

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