加速溶剂萃取-超高效液相色谱串联质谱法测定水产品中微囊藻毒素  

Determination of microcystins in aquatic products by accelerated solvent extraction coupled with ultra performance liquid chromatography-mass spectrometry

作　　者：张玲玲 虞锐鹏[2] 陶冠军[2] 王利平[2] 吴胜芳[2] 宋启军 

机构地区：[1]江南大学化学与材料工程学院,无锡214122 [2]江南大学食品科学与技术国家重点实验室,无锡214122

出　　处：《分析试验室》2016年第5期604-607,共4页Chinese Journal of Analysis Laboratory

基　　金：江南大学国家重点基本科研自主研究基金(2060204SKLF-ZZB-201507)资助

摘　　要：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。A method for rapid extraction and determination of microcystins in aquatic products by accelerated solvent extraction（ ASE） coupled with ultra performance liquid chromatography-mass spectrometry（ UPLC-MS）was proposed. Through the screening and optimization of experimental conditions,the results showed that the optimum condition for extraction was as follow： 85% methanol aqueous solution as solvent, extraction temperature of 85 ℃,static loop of two times and final extraction volume of 20 m L. Experimental results proved that peak area and concentration of the microcystins had good linear relationship in a range between 0. 025 and8 μg / g（ R2〉 0. 997）. The detection limits were between 3. 2 and 10. 0 μg / kg. The recoveries for spiked samples were in the range from 68. 5% to 86. 3%,the relative standard deviations were from 7. 0% to 9. 8%.

关 键 词：加速溶剂萃取 微囊藻毒素 水产品 超高效液相色谱-串联质谱 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]