超高效液相色谱-四极杆-飞行时间质谱法快速测定水产品中微囊藻毒素和节球藻毒素  

Determination of microcystins and nodularins in aquatic products by ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry

作　　者：虞锐鹏[1,2] 陶冠军[1,2] 杨健[1] 陈海燕[3] 徐夏叶[2] 

机构地区：[1]中国水产科学研究院内陆渔业环境与资源重点开放实验室,中国水产科学研究院淡水渔业研究中心,无锡214081 [2]江南大学食品科学与技术国家重点实验室,无锡214122 [3]宁波市鄞州区疾病预防控制中心,宁波315100

出　　处：《分析试验室》2012年第1期80-83,共4页Chinese Journal of Analysis Laboratory

基　　金：中国水产科学研究院重点开放实验室开放基金(No.YZ2009-05);宁波市自然科学基金项目(2010A610041)资助

摘　　要：通过超声提取、固相萃取纯化、超高效液相色谱-四极杆-飞行时间质谱(UPLC-Q-TOF-MS)联用技术快速测定水产品中的微囊藻毒素-RR、-YR、-LR和节球藻毒素。分别采用选择离子监测质荷比(m/z)为519.84、1045.66、995.67、825.54分子离子峰进行定量分析。该法检出限为5.0～10.0μg/kg,在浓度0.02～5 mg/kg的范围内,峰面积与样品浓度呈良好线性关系;4种藻毒素的回收率为76.2%～93.7%,相对标准偏差为2.0%～7.1%。采用上述方法对45个太湖水产品样品进行测定,发现有少量水产品中存在藻毒素污染,其中微囊藻毒素-RR最高含量为15.2μg/kg,微囊藻毒素-LR最高含量为0.84μg/kg,MC-YR、节球藻毒素均未检出。此方法可作为监测水产品体内蓄积藻毒素的分析方法。In this paper,a new analytical method,based on ultrasonic extraction and solid phase extraction,the ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry（UPLC-Q-TOF-MS） was developed for the determination of cyanotoxins in aquatic products.The protonated molecules m/z 519.84,1045.66,995.67,825.54 were selected in the selected ion monitoring mode for specific measurement of microcystin（MC） variant-RR,-YR,-LR and nodularin.The limits of detection as low as 5.0～10.0μg/kg with linear range between 0.02 and 5 mg/kg were achieved for four cyanotoxins.The recoveries for spiked samples were in the range of 76.2%～93.7% with RSDs between 2.0% and 7.1%.45 aquatic products of the Taihu lake were determined,it was found that the concentration of.MC-RR and MC-LR observed were as high as 15.2 and 0.84 μg/kg dry weight,and the contents of cyanotoxins in MC-YR and nodularin were below the limit of detection in all samples.The method is highly selective and sensitive for measurements of MCs and is adequate for analysis of MCs in aquatic products.

关 键 词：超高效液相色谱-四极杆-飞行时间质谱 水产品 微囊藻毒素 节球藻毒素 

分 类 号：O657.63[理学—分析化学]