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Alternative Liquid–Liquid Microextraction as Cleanup for Determination of Neonicotinoid Pesticides Prior HPLC Analysis

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Abstract

A simple microextraction, namely low-density solvent with low-toxicity organic solvent-based dispersive liquid–liquid microextraction (LDS-DLLME) and modified QuEChERS sample preparation procedures were optimized and validated for preconcentration of neonicotinoid pesticides prior to the determination using HPLC. The experimental parameters affecting the extraction efficiency, including salt addition, type of disperser solvent and its volume, effect of extraction solvent and its volume, and extraction time were investigated. Under the selected LDS-DLLME and HPLC conditions, separation of seven neonicotinoid pesticides (imidacloprid, acetamiprid, clothianidin, thiacloprid, thiamethoxam, dinotefuran, and nitenpyram) was achieved within 26 min. 1-Octanol (extraction solvent) and acetonitrile (disperser solvent) were used for extraction of the target analytes. Under the optimum condition, linearity was obtained within the range of 0.1–1000 ng g−1 with a correlation coefficient more than 0.999. The high enrichment factor of the target analytes was 50-fold and a low limit of quantitation (0.80–2.50 ng g−1) could be obtained. The fruit samples (at fortified levels of 10, 30, and 50 ng g−1) were successfully analyzed, and relative recoveries were obtained in the range of 90.07–112.22 %.

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Acknowledgments

This article is dedicated to Professor Dr. Kate Grudpan (Chiang Mai University, Thailand) in celebration of his 60th birthday. The authors gratefully acknowledge the financial supports of this research by the Thailand Research Fund (TRF) and Mahasarakham University, through the TRF Grant for New Scholars (Grant no. TRG5780060). The authors also gratefully acknowledge the partial supports for this research from the Center for Innovation in Chemistry (PERCH-CIC), Commission on Higher Education, Ministry of Education, and Materials Chemistry Research Center, Khon Kaen University.

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Correspondence to Jitlada Vichapong.

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Vichapong, J., Burakham, R. & Srijaranai, S. Alternative Liquid–Liquid Microextraction as Cleanup for Determination of Neonicotinoid Pesticides Prior HPLC Analysis. Chromatographia 79, 285–291 (2016). https://doi.org/10.1007/s10337-016-3022-3

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