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采用基于浮式有机液滴的分散液液微萃取与气相色谱-电子捕获检测联用技术测定桃汁、果肉和果皮中的多残留水平。

Quantification of multi-residue levels in peach juices, pulps and peels using dispersive liquid-liquid microextraction based on floating organic droplet coupled with gas chromatography-electron capture detection.

机构信息

Key Laboratory of Pesticide and Chemical Biology, Ministry of Education, College of Chemistry, Central China Normal University, Wuhan, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jul 15;879(22):2113-8. doi: 10.1016/j.jchromb.2011.05.047. Epub 2011 Jun 12.

DOI:10.1016/j.jchromb.2011.05.047
PMID:21703950
Abstract

In this paper, polychlorinated biphenyl (PCB), organochlorine pesticide (OCP) and pyrethroid pesticides in peach was investigated by comparing their residual level in peach juice, pulps and peels using dispersive liquid-liquid microextraction based on solidification of floating organic droplet (DLLME-SFO) combined with gas chromatography-electron capture detection (GC-ECD). Extraction conditions such as the type of extractant, volume of extractant and dispersant, salt effect and extraction time were optimized. For juice samples, the linearity of the method was obtained in the range of 10-2000 ng L(-1),with determination coefficients>0.99. The limits of detection (LOD) of the method were ranged between 2.8 and 18.5 ng L(-1). For pulp and peel samples, the developed method is linear over the range assayed, 1-20 μg kg(-1),with coefficients also >0.99. The relative recoveries of compounds analyzed from juice, pulp and peel samples were in the range of 73-106% with a relative standard deviation between 2.6 and 11.8%. The proposed method was applied to the simultaneous analysis of residues in real peach juice, pulp and peel samples. As a result, there were no target analytes found in peach juices and pulps while 3.3 μg kg(-1) cyhalothrin and 3.5 μg kg(-1) fenvalerate were found in peels. The experiment results revealed that the pyrethroid residues just deposited on the peels of the fruits, but did not move into pulps and juices.

摘要

本文通过比较桃汁、果肉和果皮中多氯联苯(PCB)、有机氯农药(OCP)和拟除虫菊酯类农药的残留水平,采用基于固-浮萃取分散液相微萃取(DLLME-SFO)与气相色谱-电子捕获检测(GC-ECD)相结合的方法,研究了桃中这些农药的残留情况。优化了萃取条件,如萃取剂类型、萃取剂和分散剂体积、盐效应和萃取时间。对于果汁样品,该方法在 10-2000ng/L 范围内呈线性,相关系数>0.99。方法的检出限(LOD)在 2.8-18.5ng/L 之间。对于果肉和果皮样品,所建立的方法在测定范围内呈线性,1-20μg/kg,相关系数也>0.99。化合物从果汁、果肉和果皮样品中的相对回收率在 73-106%之间,相对标准偏差在 2.6-11.8%之间。该方法被应用于实际桃汁、果肉和果皮样品中残留的同时分析。结果表明,桃汁和果肉中未检出目标分析物,而果皮中检出 3.3μg/kg 的氯氟氰菊酯和 3.5μg/kg 的氰戊菊酯。实验结果表明,拟除虫菊酯残留物仅沉积在果实的果皮上,而未转移到果肉和果汁中。

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