芯片液相色谱-质谱法高灵敏度检测水产品中微囊藻毒素

建立了一种芯片液相色谱-高分辨质谱测定3种微囊藻毒素（MC-RR、MC-YR和MC-LR）的分析方法.在最优条件下，3种藻毒素在16 min内实现基线分离，并选择电喷雾源正离子模式进行质谱测定.方法在2.5~2 000 ng/mL范围内线性良好，线性相关系数大于0.996 5，检测限介于0.5~2.0 ng/mL之间.鱼肉和虾肉样品经固相萃取法净化处理后未测得上述毒素残留，加标回收率为82.8%~120.3%.方法具有样品用量少、定性快速准确、灵敏度高等优点，适合用于水产品等生物样品中藻毒素的痕量监测.

Sensitive Analysis of Microcystins in Aquatic Products by Nano-Flow Chip Liquid Chromatography-Mass Spectrometry

A method for the simultaneous analysis of 3 microcystins (MC-RR, MC-YR and MC-LR) was set up by the nano-flow chip liquid chromatography-high resolution mass spectrometry. Under optimal conditions, the mentioned microcystins were baseline separated in 16 min with an ESI source in the positive ion mode. Good linear range in 2.5~2 000 ng/mL was obtained, with the correlation coefficient larger than 0.996 5 and the limit of detection between 0.5~2.0 ng/mL. Solid phase extraction method was used for the extraction and clean-up of fish and shrimp samples. No residue of the three microcystins was detected and the spiked recoveries were between 82.8%~120.3%. The developed method is sensitive, rapid and exact with low sample consumption, so it is reliable for the trace determination of microcystins in biological samples including aquatic products.