Liquid Chromatographic MS/MS Analysis of a Large Group of Insecticides in Honey by Modified QuEChERS

Abstract

The analytical tool for analysis of pesticide residues in honey must still be improved. Therefore, a sensitive, selective, rapid, and reliable analytical method for the analysis of pesticide residue belonging to 29 different classes at very low concentration levels was developed. Over 130 insecticides were extracted from the honey matrix using different amounts of sample, concentrations of the extraction solvent, and cleanup sorbents. Acceptable extraction recoveries accounting for matrix effect were obtained using the cleanup sorbent combination chitosan/aluminum oxide/C8 (200/200/200 mg) and 1% FA in ACN. Determinations were made by liquid chromatography-tandem mass spectrometry (LC-MS/MS). For most compounds, the recoveries range from 70 to 120%, with relative standard deviations < 20%. Linear correlation coefficients (r2) were higher than 0.99 at concentration levels of 0.001-0.100 mg kg−1. A positive matrix effect was observed for up to 95% of organophosphates and 43% of pyrethroids and a negative effect for 37% of neonicotinoids. This work showed that the presented method is convenient and reliable for quick monitoring of insecticides in honey samples.

Optimization of Method for Pesticide Detection in Honey by Using Liquid and Gas Chromatography Coupled with Mass Spectrometric Detection

“…The QuEChERS method was applied for pesticide extraction in honey by other authors [ 26 , 27 , 28 , 29 , 30 , 41 , 42 ]. The LC-MS/MS method described by Souza Tette et al [ 28 ] was validated to measure 116 pesticides in honey, but 11 compounds showed recoveries at 0.010 mg/kg out of the 70–120% range.…”

“…However, the LOD was not reported, and some pesticides showed recoveries out of the 70–120% range [ 30 ]. In another LC-MS/MS method [ 29 ], 132 tested compounds were measured in honey, obtaining recoveries ranging from 70% to 120% for 116 compounds. However, the LOD and LOQ were not provided in the manuscript nor supplementary material [ 29 ].…”

“…In another LC-MS/MS method [ 29 ], 132 tested compounds were measured in honey, obtaining recoveries ranging from 70% to 120% for 116 compounds. However, the LOD and LOQ were not provided in the manuscript nor supplementary material [ 29 ]. The GC-MS/MS method described by Zheng et al [ 41 ] was validated to measure six pesticides in honey.…”

“…Compared to earlier procedures, this method reduces the volume of solvents, and offers practical performance. Modifications of the QuECHERS method have been used for the detection of pesticides in different matrices such as meat [ 23 ], fish [ 24 ], milk [ 25 ], and honey [ 3 , 26 , 27 , 28 , 29 , 30 , 31 ].…”

“…Simultaneous detection of the residual levels of several pesticides in honey is mandatory in several countries to inspect this food before commercialization. Multi-residue analysis of at least one hundred pesticides in honey has been achieved using LC and GC coupled to mass spectrometric (MS) or tandem mass spectrometric (MS/MS) detection [ 1 , 3 , 26 , 27 , 28 , 29 , 30 , 31 , 32 ].…”