高效液相色谱串联质谱法测定鲢鱼中的微囊藻毒素

Determination of microcystins in fish by high performance liquid chromatography-tandem mass spectrometry

建立了高效液相色谱/串联质谱法(HPLC-MS/MS)同时定量检测洪泽湖鲢鱼中微囊藻毒素(MC-RR,MC-LR和MC-YR)的方法,用甲醇提取鲢鱼肉中的微囊藻毒素,用C18固相萃取柱净化。以甲醇和0.1%的甲酸水溶液为流动相,采用梯度洗脱用C18色谱柱对鱼肉中的微囊藻毒素进行分离,用电喷雾质谱正离子选择模式进行检测。三种微囊藻毒素MC-RR,MC-LR,MC-YR的线性良好,检出限分别为0.2、0.4、0.4μg·L-1,定量限分别为0.8、0.9、0.9μg·L-1。对链鱼样品进行加标回收,回收率在87.1%～101.2%,10次平行测定的相对标准偏差均小于8%。该方法具有准确、快速、简单以及灵敏度高的特点,能够适应大规模样品的快速分析要求。

Microcystins（MC-RR,MC-LR and MC-YR）were determined by high performance liquid chromatography（HPLC）combined with electrospray ionization and tandem mass spectrometry（ESI-MS/MS）. Microcystins were extracted with methanol from fish,and purified by solid-phase extraction on the C18 cartridge column. Chromatographic separation was performed on C18 column with methanol and 0. 1% of formic acid solution as mobile phase,gradient elution with using C18 column separated the microcystins from fish samples,by electrospray mass spectrometry choice model for testing. The working curves for MC-RR,MC-LR,MC-YR were good linearity,and the method detection limit were 0. 2,0. 4,0. 4μg·L-1,and quantization limits were 0. 8,0. 9,0. 9μg·L-1. The recovery rates for microcystins in fish samples were 87. 1%～101. 2%,and 10 parallel determination of the relative standard deviation was less than 8%. This method was rapid,simple and accurate,high sensitivity for measurements of MCs. It could adapt to quick analysis the large samples.