Abstract

In the present work, we developed a simple and rapid sample preparation method for the determination of neonicotinoid pesticides in honey based on the matrix-induced sugaring-out. Since there is a high concentration of sugars in the honey matrix, the honey samples were mixed directly with acetonitrile (ACN)-water mixture to trigger the phase separation. Analytes were extracted into the upper ACN phase without additional phase separation agents and injected into the HPLC system for the analysis. Parameters of this matrix-induced sugaring-out method were systematically investigated. The optimal protocol involves 2 g honey mixed with 4 mL ACN-water mixture (v/v, 60:40). In addition, this simple sample preparation method was compared with two other ACN-water-based homogenous liquid-liquid extraction methods, including salting-out assisted liquid-liquid extraction and subzero-temperature assisted liquid-liquid extraction. The present method was fully validated, the obtained limits of detection (LODs) and limits of quantification (LOQs) were from 21 to 27 and 70 to 90 μg/kg, respectively. Average recoveries at three spiked levels were in the range of 91.49% to 97.73%. Precision expressed as relative standard deviations (RSDs) in the inter-day and intra-day analysis were all lower than 5%. Finally, the developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected.

Highlights

  • Honey is a natural and healthy sweetener, which has been widely used for both nutritional and medical purposes [1]

  • The developed method was applied for the analysis of eight honey samples, results showed that none of the target neonicotinoid residues were detected

  • We aim to demonstrate that this matrix-induced phase separation phenomenon can be applied for the pretreatment of the honey sample for the determination of three typical neonicotinoid residues

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Summary

Introduction

Honey is a natural and healthy sweetener, which has been widely used for both nutritional and medical purposes [1]. Since the production of honey is inextricably linked with environment and beekeeping practices, honey could be contaminated from a variety of sources [2]. Pesticide contaminants from crops and beehives have gained great attention because of their potential to harm the health of human and honeybee [3]. Neonicotinoid pesticides are extensively used in agriculture due to their distinct characters, such as high efficacy, long-lasting effect, and superb plant-systemic activity [4]. Neonicotinoid pesticides are widely applied in seed dressings [4]. These can result in the presence of neonicotinoid residues in plant pollen or nectar. Exposure of honeybee and beehive products to neonicotinoid pesticides are envisaged [5]

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