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Preparation of a novel restricted access material combined to molecularly imprinted polymer for selective solid-phase extraction and gas chromatography determination of heptachlor, endosulfan and their metabolites residues in pork

Abstract

A novel method was established using a restricted access material combined to molecularly imprinted polymer (RAM-MIP) as sorbent material in solid phase extraction (SPE) for clean-up ofα-endosulfan, β-endosulfan, endosulfate, endosulfan-ether, endosulfan lacton, heptachlor, heptachlor-exo-epoxide, heptachlor-endo-epoxide in pork and gas chromatography (GC) for determination. RAM-MIP was prepared with precipitation polymerization by using endosulfan as template, methamylic acid (MAA) as monomer, glycidil methacrylate (GMA) as pro-hydrophilic co-monomer, ethyleneglycol dimethacrylate (EGDMA) as crosslinker, azodiisobutyronitrile (AIBN) as initiator, and toluene as porogen. Ultraviolet spectrometry (UV) and 1H-nuclear magnetic resonance (1H-NMR) analysis verified that MAA interacted specifically with endosulfan with a ratio of 1:1 in the pre-polymerization solution. RAM-MIP exhibited specific adsorption performance for endosulfan and efficiently avoided the deposition of macromolecules on the surface of polymers. The residues of endosulfan,heptachlor and their metabolites in pork were extracted with acetone: n-hexane (2:8, v/v), cleaned up by SPE cartridge packed with RAM-MIP, and determined by GC. The limits of quantification (LOQ) for endosulfan, heptachlor and their metabolites in pork samples were confined to 0.005 mg kg-1. The recoveries of target compounds spiked at 0.005-0.05 mg kg-1 were 51.17-107.73% with the relative standard deviations (RSDs) 1.4-15.9%. Thus, this novel method can be successfully applied to the determination of heptachlor, endosulfate and their metabolites residues in pork samples

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Publication details

The article was received on 09 Aug 2017, accepted on 26 Sep 2017 and first published on 27 Sep 2017


Article type: Paper
DOI: 10.1039/C7AY01941F
Citation: Anal. Methods, 2017, Accepted Manuscript
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    Preparation of a novel restricted access material combined to molecularly imprinted polymer for selective solid-phase extraction and gas chromatography determination of heptachlor, endosulfan and their metabolites residues in pork

    H. G. Zuo, Y. Hong, J. Zhu and Y. Ding, Anal. Methods, 2017, Accepted Manuscript , DOI: 10.1039/C7AY01941F

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