Analysis of Spinosad in Animal and Fishery Products by LC-MS

Abstract

We investigated the determination of spinosyn A and spinosyn D, the active ingredients of spinosad, in animal and fishery products by liquid chromatography with mass spectrometry (LC-MS). The sample was homogenized with 1 mol/L dipotassium hydrogenphosphate aqueous solution and extracted with acetone῍n-hexane under mildly alkaline conditions. After n-hexane῍ acetonitrile partitioning using an EXtrelut ῌ column, the extract was cleaned up on a tandem SAX/PSA mini-column, and examined by means of fragmenter-voltage-switching ESI-SIM mode LC-MS. Mean recoveries (n̮5)

Determination of spinosad at trace levels in bee pollen and beeswax with solid-liquid extraction and LC-ESI-MS

“…To the best of our knowledge, no research has been published in which spinosad or its active ingredients (spinosyns) have been analyzed in corbicular bee pollen or beeswax. In fact, these compounds have been studied in only one bee matrix, honey , and the methods described in such research were not exclusively aimed at analyzing residues of them in honey, but rather in several matrices , or together with other pesticides . Moreover, one study also reports the analysis of these compounds in flower pollen and plant tissues with other foliar insecticides .…”

“…For these reasons, the use of solid‐ and liquid‐phase microextraction in their different modes , quick, easy, cheap effective, rugged, and safe methods , matrix solid dispersion, and stir bar sorptive extraction have becomevery popular for the determination of pesticides in complex matrices. Some of these sample treatments have been employed to determine spinosad and its active ingredients such as liquid–liquid extraction and SLE , although reflux‐extraction methods and quick, easy, cheap effective, rugged, and safe have also been used. Diverse solvents such as hexane , dichloromethane , acetonitrile , methanol , acetone , and water were selected to extract this biopesticide.…”

“…Some of these sample treatments have been employed to determine spinosad and its active ingredients such as liquid–liquid extraction and SLE , although reflux‐extraction methods and quick, easy, cheap effective, rugged, and safe have also been used. Diverse solvents such as hexane , dichloromethane , acetonitrile , methanol , acetone , and water were selected to extract this biopesticide. It should be also mentioned that cartridges and columns have been used in some of these publications for clean‐up .…”

“…Diverse solvents such as hexane , dichloromethane , acetonitrile , methanol , acetone , and water were selected to extract this biopesticide. It should be also mentioned that cartridges and columns have been used in some of these publications for clean‐up .…”

“…LC using C 18 ‐based analytical columns has mainly been used to determine spinosyns , despite the fact that immunochemical analysis and GC have likewise been employed. Furthermore, use has been made of several detectors such as UV, diode array (DAD) , and MS to determine spinosyns in several matrices. However, MS was selected in all the studies in which honey and flower pollen were analyzed.…”