Matrix solid-phase dispersion extraction of organophosphorus pesticides from propolis extracts and recovery evaluation by GC/MS

Abstract

Five organophosphorus pesticides (dichlorvos, diazinon, malathion, methyl parathion and coumaphos) were extracted from propolis by matrix solid-phase dispersion (MSPD) extraction using octadecylsilica (C18, 1.0 g) as dispersant material. The kind of solvent elution (acetonitrile or ethyl acetate), volume (8 mL and 15 mL), and adsorbent used to clean-up the extracts (graphitized carbon, florisil™ and silica) were optimized using fortified propolis samples (5.0 μg g(-1)). Recovery was determined by gas chromatography with mass spectrometric detection in selected ion monitoring mode (GC/MS-SIM) and statistical analysis was done to determine better extraction conditions. Relatively high recovery and lower relative standard deviation values (3.1-14.6%) were obtained when analytes were eluted with ethyl acetate from the MSPD column. Diazinon, malathion, methyl parathion, and coumaphos show recoveries of 72.7%, 84.6%, 62.6%, and 78.3%, respectively. In contrast, the recovery for dichlorvos was 53.8%. Additional adsorbents tested for clean-up and increase in solvent elution did not affect recoveries positively and caused a high background in chromatograms. Thus, final conditions were 1 mL of sample, 1 g C18 and 8 mL of ethyl acetate.

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

“…Primary secondary amine (PSA) and graphitized carbon (GCN) were tested as co-columns for the clean up step because of their strong affinities for pigments (chlorophyll, carotenoids), sterols, sugars, fatty acids, and other compounds [31]. In general, with PSA and GCN, the MSPD extracts were cleaner (no color) than those obtained without co-columns; this agrees with our previous work on organophosphorus pesticides in propolis [29].…”

“…Based on previous work [29], the combination of a nonpolar solid support (C18) and a polar solvent (ACN) was selected for MSPD extraction. In particular, due to its lipophilicity, C18 is suitable for extracting analytes from samples with high lipid contents [30].…”

Propolis Counteracts Some Threats to Honey Bee Health

“…There is limited evidence that acaricides can occasionally be found in propolis collected from a hive [22,117,118], as well as the antibiotic (tylosin) used to treat the bacterial diseases American foulbrood and European foulbrood (two of 30 samples from China had detectable amounts [119]). Similarly low levels of pesticide residues likely from treatments on the plant sources or contaminated pollen have been detected in some propolis samples [120,121], but not in others [122,123]. Further study on the frequency and abundance of these chemicals in propolis samples needs to be conducted as well as the possible antagonistic effect that these compounds could have on the chemical constituents of propolis or possibly the synergistic effects that the residues have with those chemicals found in wax, honey and pollen stores (i.e., [124,125]).…”

Microwave Assisted Head Space Solid Phase Microextraction for Analysis of Butachlor and Chlorpyrifos Pesticides in Urine

“…Therefore, a rapid, accurate, and sensitive method is required for biological monitoring of these pesticides. Several analytical techniques have been developed for sample preparation to facilitate identification of pesticides from biological and environmental samples including Liquid-liquid extraction (LLE) 10,13 , solid-phase extraction (SPE) 14 , supercritical fluid extraction (SFE) 15 and matrix solid-phase dispersion (MSPD) 16 . Generally, these methods are multistage, expensive, laborious, and take long time to be performed and require large volume of solvents 17 .…”