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[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。
[Objective] The research aimed to establish a method for simultaneous determination of seven microcystin (MC) in aquatic products by high performance liquid chromatography-tandem mass spectrometry. [Method] The samples were extracted with buffer of Tris-HC (lpH = 7), purified with Oasis HLB, separated by C18 column, detected by electrospray ionization mass spectrometry and quantified by internal standard method. [Result] The seven microcystins MC-LR, MC-RR, MC-YR, MC-LA, MC-LW, MC-LY and MC-LF in aquatic products could be completed simultaneously by effective extraction and purification The recoveries of 10 μg / kg and 40 μg / kg in 4 different aquatic products were 51% ~ 112% and 60% ~ 117% with RSDs of 1.7% ~ 12.7% and 0.9% ~ 8.0% n = 6). The detection limit was 0.20 ~ 0.40μg / kg. [Conclusion] Simultaneous determination of seven microcystins in aquatic products by liquid chromatography-tandem mass spectrometry established in this study was a rapid, effective and practical method for the determination of microcystin residues in aquatic products. The microcystin monitoring provides a strong technical support.