[Analysis of spinosad in animal and fishery products by LC-MS].
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.
Aichi Prefectural Institute of Public Health, Nagoya, Japan.
Eiji
E
Ueno
Haruka
H
Ohno
Minae
M
Watanabe
Harumi
H
Oshima
Eiichi
E
Mikami
Satoru
S
Nemoto
Rieko
R
Matsuda
D000818:Animals; D002417:Cattle; D002645:Chickens; D002853:Chromatography, Liquid / Q000379:methods*; D004338:Drug Combinations; D004531:Eggs / Q000032:analysis*; D005504:Food Analysis / Q000379:methods*; D005506:Food Contamination / Q000032:analysis*; D006722:Honey / Q000032:analysis*; D007306:Insecticides / Q000032:analysis* / Q000302:isolation & purification; D018942:Macrolides / Q000032:analysis* / Q000302:isolation & purification; D013058:Mass Spectrometry / Q000379:methods*; D008461:Meat Products / Q000032:analysis*; D008892:Milk / Q000737:chemistry*; D010573:Pesticide Residues / Q000032:analysis*; D017747:Seafood / Q000032:analysis*
D004338:Drug Combinations; D007306:Insecticides; D018942:Macrolides; D010573:Pesticide Residues; C415329:spinosad