Abstract

Article history: Received July 21, 2015 Received in revised form August 29, 2015 Accepted 19 September 2015 Available online 20 September 2015 This paper describes a harmless HPLC technique for detecting imidacloprid (ICP) and its metabolite, 6-chloronicotinic acid (6CA), using an isocratic 100 % water mobile phase. Chromatographic separations were performed a Daisopak® SP-200-3-C1-P with water mobile phase and a photodiode-array detector. The total run time was < 6 min. The system suitability was well within the international acceptance criteria. The detection limits were 0.018 μg/ml for ICP and 0.005 μg/ml for 6CA, respectively. A harmless HPLC method for simultaneous detecting ICP and 6CA was developed and may be further applied to the quantification in animal-derived foods. © 2015Growing Science Ltd. All rights reserved.

Highlights

  • Overuse of pesticides is always associated with risk of food residues

  • This paper describes a harmless HPLC technique for detecting imidacloprid (ICP) and its metabolite, 6-chloronicotinic acid (6CA), using an isocratic 100 % water mobile phase

  • The first is oxidative cleavage, yielding 6-chloronicotinic acid (6CA) (Fig. 1), which is conjugated with glycine to form a hippuric acid-type conjugate

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Summary

Introduction

Overuse of pesticides is always associated with risk of food residues. In December 2013, imidacloprid (1-(6-chloro-3-pyridylmethyl)-N-nitroimidazolidin-2-ylideneamine) (ICP) (Figure 1), a widely/frequently-used neonicotinoid insecticide, may affect the developing human nervous system, disclose the European Food Safety Authority. Previous techniques based on high-performance liquid chromatographic (HPLC) combined with UV, photo-diode array (PDA), MS, and MS/MS for the monitoring ICP and 6CA4-6 have crucial drawbacks: 1) all of the methods consume large quantities of toxic organic solvents, acetonitrile and/or methanol,[7] in the mobile phases. Risk associated with these solvents extend beyond direct implications for the health of humans and wildlife to affect our environment and the ecosystem in which we all reside. As the first examination problem in the establishment of an international harmonized method for the residue monitoring of ICP and 6CA, this paper describes an isocratic 100 % water mobile phase HPLC conditions to detect ICP and 6CA

Optimum HPLC conditions
HPLC validation
Conclusions
Experimental
Operating conditions
Preparation of Stock Standards and Working Mixed Solutions
System suitability test
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