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

Determination of 7 Microcystin Variants in Aquatic Products by High Performance Liquid Chromatography-Tandem Triple Quadrupole Mass Spectrometry

[目的]建立用高效液相色谱一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．HCl（pH=7）缓冲液提取、HLB固相萃取柱（OasisHLB）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、40tc／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一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 ] To establish a high performance liquid chromatography-tandem triple quadrnpole mass spectrometry method for simultaneous determination of 7 variants of mierocystins in aquatic products. [ Methods ] All samples were subject to extraction in Tris-HC1 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 mieroeystins of LR, RR, YR, LA, LW, LY and LF were detected simultaneously. The mean recoveries spiked at levels of 10 μg/kg and 40 μg/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）, respeetiveIy. The limits of detection were 0.20-0.40 μg/kg. [ Conclusion ] A rapid and practical method with high efficiency is proposed and provides technical basis for standard determination protocol of mierocystins.