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Effectiveness of different cleanup sorbents for the determination of avermectins in fish by liquid chromatography tandem mass spectrometry

机译:液相色谱串联质谱法测定不同净化吸附剂测定鱼中阿维菌素的有效性

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An effectiveness and comparative study of cleanup sorbents used in dispersive solid phase extraction (DSPE) for the determination of avermectins, including emamectin (EMA), abamectin (ABA), doramectin (DOR), moxidectin (MOX), and ivermectin (IVE), was performed. Three different types of cleanup sorbents, alumina (Al), primary and secondary amine (PSA) and octadecyl (C18), were used to remove the matrix interference in fish samples. Homogenised fish samples were extracted with acetonitrile, magnesium sulphate anhydrous and sodium chloride. The cleanup sorbents were separately applied to the supernatant during the DSPE procedure; the mixtures were shaken and centrifuged, and the supernatant was dried. The extracts were reconstituted with acetonitrile/water and quantified by liquid chromatography tandem mass spectrometry with electrospray ionisation in the positive mode with two product ions that were monitored by selected reaction monitoring. The performance of each cleanup sorbent was observed for its accuracy and precision in a spiked blank sample at a concentration of 5 ??g kga?’1. The combination of the cleanup sorbents PSA and C18 was found to be the most effective in the cleanup of the fish samples. In the validation tests, the detection limit was in the range of 0.3 ??g kga?’1 to 0.4 ??g kga?’1, and the quantitation limit for all avermectins was 1 ??g kga?’1 in the linearity range of 1a€“15 ??g kga?’1. The recoveries of avermectins were 91.9a€“102.5%, with a relative standard deviation lower than 19%.
机译:分散固相萃取(DSPE)中用于测定阿维菌素的净化吸附剂的有效性和比较研究,包括阿马菌素(EMA),阿巴菌素(ABA),多拉菌素(DOR),莫昔克丁(MOX)和伊维菌素(IVE),被执行了。三种不同类型的净化吸附剂,氧化铝(Al),伯胺和仲胺(PSA)和十八烷基(C18)用于去除鱼样品中的基质干扰物。将均质的鱼样品用乙腈,无水硫酸镁和氯化钠萃取。在DSPE程序中,将清除吸附剂分别应用于上清液;摇动并离心混合物,并将上清液干燥。提取物用乙腈/水重构,并通过液相色谱串联质谱法进行定量,其中电喷雾电离为正模式,其中两种产物离子通过选定的反应监测器进行监测。观察每种净化吸附剂在加标空白样品中浓度为5 ?? g kga?-1时的准确性和精密度。发现清洁吸附剂PSA和C18的组合对鱼类样品的清洁最有效。在验证测试中,检出限为0.3 ?? g kga?'1至0.4 ?? g kga?'1,线性范围内所有阿维菌素的定量限为1 ?? g kga?'1。范围为1a“ 15千克/公斤” 1。阿维菌素的回收率为91.9a±102.5%,相对标准偏差低于19%。

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