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Fast Analysis of Synthetic Pyrethroid Metabolites in Water Samples Using In-Syringe Derivatization Coupled Hollow Fiber Mediated Liquid Phase Microextraction with GC-ECD

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Abstract

A fast and efficient method has been demonstrated for the trace determination of six important metabolites of synthetic pyrethroids including cis- and trans-3-(2,2-dichlorovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (cis- and trans-Cl2CA), cis-3-(2,2-dibromovinyl)-2,2-dimethylcyclopropane-1-carboxylic acid (cis-Br2CA), 4-fluoro-3-phenoxybenzoic acid (4-F-3-PBA), 3-phenoxybenzoic acid (3-PBA), and 2-phenoxybenzoic acid (2-PBA) in environmental water samples using hollow fiber (HF)-mediated liquid-phase microextraction (LPME) coupled with in-syringe derivatization (ISD) followed by gas chromatography (GC) with electron capture detector (ECD) analysis. This method utilizes a HF membrane segment impregnated with extraction solvent as the LPME sampling probe, which was connected to a microsyringe pre-filled with derivatizing agents, and it was immersed into sample solution for extraction. After extraction, the extracting solution was subjected to derivatization reaction that was performed inside the syringe barrel followed by GC-ECD analysis. Under optimal conditions, the best extraction efficiency was obtained using sampling probe (2.0 cm hollow fiber) impregnated with 1-octanol immersed into water sample (5.0 mL, adjusted pH below 1.0) and stirring (1,250 rpm) for 10 min at 70 °C and diisopropylcarbodiimide (2 μL) and 1,1,1,3,3,3-hexafluoro-2-propanol (1 μL) were the derivatizing agents used. The detection limits of 3 ng mL−1 for cis- and trans-Cl2CA, 2 ng mL−1 for cis-Br2CA, 6 ng mL−1 for 4-F-3-PBA, and 0.6 ng mL−1 for 3-PBA and 2-PBA. The method showed good linearity (R 2 = 0.973−0.998), repeatability from 4.0 to 13 % (n = 5), recovery from 79.2 to 95.7 %, and enrichment factors ranged between 109 and 159 for target analytes spiked in water samples. The proposed method and conventional methods were compared. Results suggested that the proposed HF-LPME-ISD/GC-ECD method was a rapid, simple, inexpensive, and eco-friendly technique for the analysis of metabolites of pyrethroids.

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Acknowledgments

The authors are thankful for financial supports from the National Science Council of Taiwan under the Grant number NSC 94-2113-M-005-002 and the Council of Agriculture (COA) in Taiwan under the Grant number 90AS-1.2.2-PI-P2(3).

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Authors and Affiliations

  1. Department of Chemistry, National Chung Hsing University, Taichung City, 402, Taiwan

    Chiu-Hwa Lin, Vinoth Kumar Ponnusamy & Jen-Fon Jen

  2. Residure Control Department, Taiwan Agricultural Chemicals and Toxic Substances Research Institute, Council of Agriculture (TACTRI/COA), Wu-Fung, Taichung City, 413, Taiwan

    Chiu-Hwa Lin & Hong-Ping Li

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  1. Chiu-Hwa Lin
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  2. Vinoth Kumar Ponnusamy
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  3. Hong-Ping Li
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  4. Jen-Fon Jen
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Correspondence to Jen-Fon Jen.

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Lin, CH., Ponnusamy, V.K., Li, HP. et al. Fast Analysis of Synthetic Pyrethroid Metabolites in Water Samples Using In-Syringe Derivatization Coupled Hollow Fiber Mediated Liquid Phase Microextraction with GC-ECD. Chromatographia 76, 75–83 (2013). https://doi.org/10.1007/s10337-012-2360-z

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  • DOI: https://doi.org/10.1007/s10337-012-2360-z

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