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芒果果肉中农药测定的能力验证:所用色谱技术概述及实验室性能评估

Proficiency testing for the determination of pesticides in mango pulp: a view of the employed chromatographic techniques and the evaluation of laboratories' performance.

作者信息

Violante F G M, Bastos L H P, Cardoso M H W M, Rodrigues J M, Gouvêa A V, Borges C N, Santos P R da F, Santos D da S, Góes H C de A, Souza V, de São José A, Bandeira R D C C, Cunha V, Nóbrega A

机构信息

Divisão de Metrologia Química, Diretoria de Metrologia Científica e Industrial Dimci, Instituto Nacional de Metrologia, Normalização e Qualidade Industrial, Duque de Caxias, RJ, Brasil.

出版信息

J Chromatogr Sci. 2009 Oct;47(9):833-9. doi: 10.1093/chromsci/47.9.833.

DOI:10.1093/chromsci/47.9.833
PMID:19835699
Abstract

The proficiency testing for determination of pesticides residues in mango pulp was the third work of the partnership established by INMETRO and INCQS/Fiocruz. Three mango pulp samples were sent to each participant laboratory, two being spiked with the pesticides and one exempt of pesticides. The added pesticides were: deltamethrin, ethion, fenitrothion, malathion, and permethrin. The evaluation of the results of the homogeneity and the stability tests, as well as the determination of the assigned value was made in agreement with ISO GUIDE 35 and ISO 13528, assuming the samples were considered homogeneous and stable for the studied period. The assigned values and the standard deviation for proficiency evaluation was calculated using the robust algorithm, according to ISO 13528, and the evaluation of the results was carried through in accordance with ABNT ISO/IEC Guide 43-1. The z-score graphs and confidence ellipse was also used in the evaluation of the results. In the evaluation carried through from the values of the z-scores, 71% of the reported results were considered satisfactory based on the results found for this index. The evaluation of the analytical viability for the determination of each pesticide and of the analytical capacity of the participant laboratories was carried through. A summarized view of the chromatographic techniques and of preparation of sample used by the participant laboratories was also carried through in this work.

摘要

芒果果肉中农药残留量的能力验证是巴西计量、标准化和工业质量局(INMETRO)与奥斯瓦尔多·克鲁兹基金会(Fiocruz)下属的国家卫生质量控制研究所(INCQS)建立的合作项目的第三项工作。向每个参与实验室发送了三个芒果果肉样本,其中两个添加了农药,一个未添加农药。添加的农药有:溴氰菊酯、乙硫磷、杀螟硫磷、马拉硫磷和氯菊酯。根据ISO指南35和ISO 13528,对均匀性和稳定性测试结果进行评估,并确定赋值,假定在所研究期间样本被视为均匀且稳定。根据ISO 13528,使用稳健算法计算能力验证的赋值和标准偏差,并按照巴西标准协会(ABNT)ISO/IEC指南43-1对结果进行评估。z分数图和置信椭圆也用于结果评估。根据该指标的结果,从z分数值进行的评估中,71%的报告结果被认为是令人满意的。对每种农药测定的分析可行性以及参与实验室的分析能力进行了评估。这项工作还对参与实验室使用的色谱技术和样品制备进行了总结。

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