Chinese Journal of Chromatography ›› 2014, Vol. 32 ›› Issue (10): 1131-1137.DOI: 10.3724/SP.J.1123.2014.07028

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Magnetic solid phase extraction combined with gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in juice samples

HUANG Qian, HE Man, CHEN Beibei, HU Bin   

  1. Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China
  • Received:2014-07-18 Online:2014-10-08 Published:2014-09-29

Abstract:

A novel method for the determination of organophosphorous pesticides (OPPs) in fresh juice samples was developed. Fe3O4@P(St-co-MAA) magnetic microparticles were synthesized and modified with styrene (St) and methacrylic acid (MAA) by coating St and MAA on magnetic particles and characterized by a series of techniques. The results indicated that Fe3O4 magnetic nanoparticles (MNPs) have been successfully modified with St and MAA. Based on the prepared Fe3O4@P(St-co-MAA) magnetic microparticles, a novel method of magnetic solid phase extraction (MSPE)-gas chromatography (GC)-flame photometric detection (FPD) was developed for the determination of OPPs. The extraction/desorption conditions of MSPE were optimized, and the analytical performance was evaluated under the optimal conditions. The limits of detection (LODs, S/N=3) for target OPPs were in the range of 0.013-0.305 μg/L with the RSDs (n=7) ranging from 3.1% to 8.8%. The enrichment factors varied from 406 to 951. The linear ranges were over three orders of magnitudes (R2>0.99) and the reproducibilities were 7.4%-14.5% (n=5). Finally, the proposed MSPE-GC-FPD method was successfully applied to the analysis of the five OPPs in fresh tomato and strawberry juice samples, with the recoveries of target OPPs in the range of 85.4%-118.9% for the spiked samples. The proposed MSPE-GC-FPD method is featured with low cost, fast separation and high enrichment factor.

Key words: gas chromatography-flame photometric detection (GC-FPD), juices, magnetic solid phase extraction (MSPE), organophosphorus pesticides (OPPs)

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