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用于测定水果和果汁中有机磷农药的固相微萃取方法的验证

Validation of a solid-phase microextraction method for the determination of organophosphorus pesticides in fruits and fruit juice.

作者信息

Simplício A L, Boas L V

机构信息

Instituto de Biologia Experimental e Tecnológica, Oeiras, Portugal.

出版信息

J Chromatogr A. 1999 Feb 12;833(1):35-42. doi: 10.1016/s0021-9673(98)00941-8.

DOI:10.1016/s0021-9673(98)00941-8
PMID:10074697
Abstract

A method for the determination of organophosphorus pesticides (diazinon, fenitrothion, fenthion, quinalphos, triazophos, phosalon and pyrazophos) in fruit (pears) and fruit juice samples was developed and validated. The samples were diluted with water, extracted by solid-phase microextraction (SPME) and analysed by gas chromatography (GC) using a flame photometric detector in phosphorous mode. Limits of detection of the method for fruit and fruit juice matrices were below 2 micrograms/kg for all pesticides. Relative standard deviations for triplicate analyses of samples fortified at 25 micrograms/kg of each pesticide were not higher than 8.7%. Recovery tests were performed for concentrations between 25 and 250 micrograms/kg. Mean recoveries for each pesticide were all above 75.9% and below 102.6% for juice, and between 70 and 99% for fruit except for pyrazophos in the fruit sample (with mean recovery of 53%). Therefore, the proposed method is applicable in the analysis of pesticides in fruit matrices and the use of the method in routine analysis of pesticide residues is discussed.

摘要

建立并验证了一种测定水果(梨)和果汁样品中有机磷农药(二嗪农、杀螟硫磷、倍硫磷、喹硫磷、三唑磷、伏杀硫磷和吡唑硫磷)的方法。样品用水稀释,通过固相微萃取(SPME)进行萃取,并用配备磷模式火焰光度检测器的气相色谱(GC)进行分析。该方法对水果和果汁基质中所有农药的检测限均低于2微克/千克。对每种农药添加浓度为25微克/千克的样品进行三次重复分析,相对标准偏差不高于8.7%。在25至250微克/千克的浓度范围内进行了回收率测试。果汁中每种农药的平均回收率均高于75.9%且低于102.6%,水果中除水果样品中的吡唑硫磷(平均回收率为53%)外,回收率在70%至99%之间。因此,所提出的方法适用于水果基质中农药的分析,并讨论了该方法在农药残留常规分析中的应用。

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