High-throughput HPLC–MS/MS determination of the persistence of neonicotinoid insecticide residues of regulatory interest in dietary bee pollen

Abstract

The aim of this work is the development of a simple, fast, quantitative, and economic method for the determination of neonicotinoid insecticide residues in dietary bee pollen. Several parameters of the method, such as extraction solvent, extraction time, and solid-phase extraction sorbents for purification [silica, C18, primary-secondary amine (PSA), and Envi-Carb II/PSA], were studied. The final proposed method based on solid-liquid extraction with hexane, cleanup with Supelclean™ Envi-Carb II/PSA cartridges, and subsequent analysis by high-performance liquid chromatography with tandem mass spectrometry was validated and applied to the analysis of commercial bee pollen samples from different geographical zones. Method performance was assessed by the evaluation of several quality parameters of the method, such as recovery values, repeatability, reproducibility, linearity, and limits of detection and quantification. Matrix effects on the chromatographic signal were also studied. The quality parameters of the method were equivalent to or better than those obtained with previously published methods, with recoveries between 81 and 99% and repeatabilities lower than 8.8%. The detection and quantification limits were in the ranges 0.2-2.2 μg kg(-1) and 0.4-4.3 μg kg(-1), respectively.

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.…”

Mass spectrometric approaches for the identification of anthracycline analogs produced by actinobacteria

“…The new anthracycline, compound 8, was isolated as a purple powder. [α] [25] D -31.49°(c 0.002, CH 3 OH). The UV spectrum displayed λ max (MeOH) at 254, 287 and 539 nm.…”

“…[22,23] Certainly that the multiple reaction monitoring, a targeted approach, is the most successful method developed in triple quadrupole, and it has been widely applied for quantitative analyses of small organic molecules as drugs, pesticides and toxins as a result of low detection limit (femtomole range). [24,25] The precursor ion scan, a focused method, is mainly used to enable the analyses of minor unknown metabolites monitoring diagnostic fragment ions by focusing in the loss of some specific group of the compounds. [23] This scan mode has been applied in structural characterization of small molecules [26] to detect metabolite derivatives in biological samples [27] in protein identification [28] and others; however, its main application is in recognition of group of compounds with specified functional groups present in complex mixtures.…”

A fluorescence polarization immunoassay for detection of thiacloprid in environmental and agricultural samples

“…Many instrument-based methods have been established to detect thiacloprid in various samples, such as highperformance liquid chromatography (HPLC), HPLC-tandem mass spectrometry, supercritical uid chromatographictandem mass spectrometry and so on. [6][7][8] However, immunoassay, with the advantages of simplicity, high sensitivity and low cost, shows greater advantage and potential than instrumentbased methods in analysis of large number of samples, 9 which has been used for detection of thiacloprid. Liu et al prepared the anti-thiacloprid polyclonal antibody to develop enzyme-linked immunosorbent assay (ELISA), 10 and used various tracers to enhanced the sensitivity, such as enhanced chemiluminescent enzyme immunoassay and time-resolved uoroimmunoassay.…”