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气相色谱法测定明胶中的五氯苯酚:协同研究

Gas chromatographic determination of pentachlorophenol in gelatin: collaborative study.

作者信息

Yip G

出版信息

J Assoc Off Anal Chem. 1985 May-Jun;68(3):419-21.

PMID:4019362
Abstract

Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1% SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.

摘要

11位合作者参与了这项关于气相色谱法测定明胶中五氯苯酚(PCP)的研究。取2g样品进行酸水解后,用己烷萃取PCP,再将其分配至氢氧化钾溶液中。重新酸化后,再次用己烷萃取PCP,通过在1% SP - 1240DA柱上的电子捕获气相色谱法进行测定。每位合作者分析了3个重复的标准样品(0.0、0.5和1.5 ppm)以及5个盲样重复协作样品(0.0、0.02、0.1、0.5和2.0 ppm)。协作样品中PCP的平均回收率在0.02 ppm加标水平下为88%,在0.1 ppm水平下为102%;总体平均回收率为96%。实验室间变异系数在0.1 ppm加标水平下为16.4%,在0.5 ppm水平下为22.9%;总体实验室间变异系数为19.5%。该方法已被首次官方采用。

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