Validation and monitoring of pesticide residues in honey using QuEChERS and gas chromatographic analysis

Abstract

A fast and simple multiresidue method for the analysis of the residues of 11 organochlorine (OC) compounds, four organophosphate (OP) compounds, four pyrethroid compounds, two herbicides, and one phenyl pyrazole pesticide in honey is presented. A useful and fast method for the separation of 22 pesticides from different organochlorine, organophosphate, and pyrethroid groups was modified and standardized using QuEChERS and GC-ECD system and used for the determination of pesticide residues in 30 samples of honey collected from the Hisar region of India. The proposed method is simple, rapid, and reliable where satisfactory recoveries were observed. The recovery values obtained at three fortification levels: 0.01, 0.25, and 0.50 mg kg⁻¹ were within the range of recommended values (70–120%), with RSDs in general below < 20%. Among organochlorines, aldrin (0.093–0.282 mg kg⁻¹) was detected in 16 samples followed by δ-HCH (0.018–0.126 mg kg⁻¹) in nine samples. Chlorpyriphos methyl (0.032–0.083 mg kg⁻¹) among the organophosphates was detected in 10 samples. Cypermethrin (0.162–0.610 mg kg⁻¹) and bifenthrin (0.190–0.344 mg kg⁻¹) among the pyrethroids were detected in two and three samples, respectively.

Se expone un método multi-residuo rápido y sencillo para analizar los residuos de 11 compuestos organoclorados (OC), cuatro organofosforados (OP), cuatro piretroides, dos herbicidas y un plaguicida fenil pirazol en la miel. Se modificó y estandarizó un método útil y rápido para la separación de 22 plaguicidas entre diferentes grupos de organoclorados, organofosforados y piretroides usando QuEChERS y GC-ECD, y se utilizó para la detección de residuos plaguicidas en 30 muestras de miel recogidas en la región de Hisar en la India. El método propuesto es simple, rápido y fiable, habiéndose observado recuperaciones satisfactorias. Los valores de recuperación obtenidos a tres niveles de enriquecimiento fueron: 0,01, 0,25 y 0,50 mg kg⁻¹y se situaron dentro del rango de valores recomendados (70-120%), con un RSDs por debajo del 20% en general. Entre los organoclorados, se detectó el aldrin (0,093-0,283 mg kg⁻¹) en 16 muestras seguido por el δ-HCH (0,018-0,224 mg kg⁻¹) en nueve muestras. Entre los organofosforados, se detectó metil clorpirifós (0,32-0,083 mg kg⁻¹) en 10 muestras. Finalmente, entre los piretroides, se detectó cipermetrina y bifentrina en 2 y 3 muestras, respectivamente.

Keywords:

• pesticides
• honey
• QuEChERS
• GC

Acknowledgments

The authors wish to express their gratitude to ICAR, New Delhi for Senior Research Fellowship to Dr. Hasansab A. Nadaf and the Head, Department of Entomology for providing research facilities. We are grateful to Dr S. K. Sharma, Dr H. D. Kaushik, and Dr Yogesh kumar for their thoughtful discussion and suggestion. We thank the beekeepers of the Hisar region for their help in sample collection.