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采用加速溶剂萃取(ASE)和超高效液相色谱-串联质谱(UPLC-MS)联用技术,建立了快速提取和测定水产品中微囊藻毒素MC-RR、MC-LR的方法。通过对实验条件的筛选和优化,确定ASE的优化条件:85%甲醇水溶液为萃取剂,弗罗里硅土为吸附剂,温度85℃,静态循环2次,最终萃取体积20 m L。微囊藻毒素的质量分数在0.025~8μg/g范围内,峰面积与样品质量分数线性关系良好(R~2>0.997),检出限为3.2~10.0μg/kg。样品加标回收率为68.5%~86.3%,相对标准偏差在7.0%~9.8%之间。
The rapid extraction and determination of microcystins MC-RR and MC-LR in aquatic products were established by the combination of accelerated solvent extraction (ASE) and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS). Through the screening and optimization of experimental conditions, the optimal conditions of ASE were determined: 85% methanol aqueous solution as extractant, Florisil as adsorbent, 85 ℃ static cycle and 2 final extraction volume of 20 mL. The mass fraction of microcystin was in the range of 0.025-8μg / g, and the peak area was linear with the sample mass fraction (R ~ 2> 0.997). The detection limit was 3.2-10.0μg / kg. The recoveries of spiked samples ranged from 68.5% to 86.3% with relative standard deviations between 7.0% and 9.8%.