Extraction of Organochlorine Pesticides from Bee Pollen by Matrix Solid-Phase Dispersion: Recovery Evaluation by GC–MS and Method Validation

Abstract

Recovery studies were done with bee pollen spiked with eight organochlorine pesticides. Matrix solidphase dispersion was used to extract pesticides from bee pollen using octadecyl silica (C18, 0.5 g) as solid support. The co-column material for clean-up (graphitized carbon and primary secondary amine) and the eluting system (acetonitrile or acetonitrile/ethyl acetate) were optimized. Pesticide recoveries were determined by GC-MS-SIM through external calibration curves. The recoveries obtained without co-column and primary secondary amine (PSA) did not differ significantly and were higher than those obtained using graphitized carbon. With PSA used as the co-column, chromatograms with low background, low intensity, and fewer peaks were acquired. Thus, primary secondary amine was used to clean up the pollen extracts. Recoveries were higher than 100 % and precisions were poor for most of the pesticides when acetonitrile/ethyl acetate was used to elute them. Therefore, acetonitrile was selected for the elution of organochlorine pesticides. The final extraction conditions were: C18 (adsorbent), primary secondary amine (co-column), and ACN (eluting solvent). Recoveries obtained ranged from 41 to 101 %.

Miniaturized Salting-Out Assisted Liquid-Liquid Extraction Combined with Disposable Pipette Extraction for Fast Sample Preparation of Neonicotinoid Pesticides in Bee Pollen

“…Because of the complexity of the constituents in bee pollen, sample preparation to extract and clean up target compounds is generally required when chromatography-based technology is employed for the analysis of pesticide residues [5]. Classical solid-liquid extraction [6], solid-phase extraction (SPE) [7,8], matrix solid-phase dispersion (MSPD) [9], and dispersive solid-phase extraction (d-SPE) [10][11][12] methods have been developed for the determination of pesticides in bee pollen. Despite this progress, it is still a great challenge to develop a simple and rapid sample preparation method for residue analysis in bee pollen matrix.…”

Determination of multiclass pesticides in river sediments via matrix solid‐phase dispersion extraction and gas chromatography–tandem mass spectrometry

“…Although Barker et al [17] initially introduced the technique to extract drugs in bovine muscle, MSPD has spread and found application to extract drugs, pharmaceuticals, pesticides, and many other contaminants in a wide diversity of solid or semisolid samples [18][19][20][21][22][23].…”