Ueno Eiji, Ohno Haruka, Watanabe Minae, Oshima Harumi, Mikami Eiichi, Nemoto Satoru, Matsuda Rieko
Aichi Prefectural Institute of Public Health, Nagoya, Japan.
Shokuhin Eiseigaku Zasshi. 2011;52(6):330-5. doi: 10.3358/shokueishi.52.330.
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.
我们采用液相色谱-质谱联用（LC-MS）法研究了多杀菌素的活性成分多杀菌素A和多杀菌素D在动物和渔业产品中的测定方法。样品用1 mol/L磷酸氢二钾水溶液匀浆，并在弱碱性条件下用丙酮-正己烷萃取。使用EXtrelut(®)柱进行正己烷-乙腈分配后，提取物在串联SAX/PSA微型柱上净化，并通过碎裂电压切换ESI-SIM模式LC-MS进行检测。在分析物浓度为0.01 µg/g和0.05 µg/g时，从11种加标样品中回收的多杀菌素A和多杀菌素D的平均回收率（n = 5）分别为76.1%至93.8%（RSD≤8.7%）和75.1%至104.1%（RSD≤8.6%）。
