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® 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 (n=5) of spinosyn A and spinosyn D from eleven kinds of fortified samples at the analyte concentration of 0.01 μg/g and 0.05 μg/g ranged from 76.1% to 93.8% (RSD≤8.7%) and from 75.1% to 104.1% (RSD≤8.6%), respectively.