【摘要】 [目的]建立用高效液相色谱-串联质谱法同时测定水产品中7种微囊藻毒素(microcystin,MC)的测定方法。[方法]样品经Tris-HC(lpH=7)缓冲液提取、HLB固相萃取柱(Oasis HLB)净化、C18柱分离、电喷雾电离质谱检测、内标法定量。[结果]通过有效的提取和净化,能同时完成水产品中7种微囊藻毒素MC-LR、MC-RR、MC-YR、MC-LA、MC-LW、MC-LY和MC-LF的测定,4种不同水产品基质中10μg/kg、40μg/kg加标回收率为51%~112%和60%~117%,相对标准偏差分别为1.7%~12.7%和0.9%~8.0%(n=6);检出限为0.20~0.40μg/kg。[结论]本研究建立的液相色谱-串联质谱同时测定水产品中7种微囊藻毒素的测定方法是测定水产品中微囊藻毒素残留量快速、有效、实用的方法,能为水产品中微囊藻毒素的监测提供有力的技术保障。更多还原

【Abstract】 [Objective] To establish a high performance liquid chromatography-tandem triple quadrupole mass spectrometry method for simultaneous determination of 7 variants of microcystins in aquatic products.[Methods]All samples were subject to extraction in Tris–HCl buffer(pH=7),clean-up with Oasis HLB solid phase extraction,C18 separation,mass spectrometry detection and quantification with internal standards.[Results]After effective extraction and purification,7 microcystins of LR,RR,YR,LA,LW,LY and LF were detected simultaneously.The mean recoveries spiked at levels of 10μg/kg and 40μg/kg in four matrices were 51%-112% and 60%-117%,with relative standard deviation of 1.7%-12.7% and 0.9%-8.0%(n=6),respectively.The limits of detection were 0.20-0.40μg/kg.[Conclusion]A rapid and practical method with high efficiency is proposed and provides technical basis for standard determination protocol of microcystins.更多还原