高效液相色谱-串联质谱法测定水产品中7种微囊藻毒素

Simultaneous Determination of Seven Microcystins in Aquatic Product by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法同时测定水产品中7种微囊藻毒素(微囊藻毒素-RR、微囊藻毒素-YR、微囊藻毒素-LR、微囊藻毒素-LA、微囊藻毒素-LW、微囊藻毒素-LF、微囊藻毒素-LY)的分析方法。样品用90%甲醇水(V/V)溶液提取,经离心、固相萃取柱净化后,用C18柱,以0.1%甲酸乙腈-0.1%甲酸溶液为流动相,梯度洗脱分离,使用三重四级杆质谱检测器检测,以保留时间及特征离子对定性,外标法定量。结果表明,7种微囊藻毒素在线性范围内线性关系良好,相关系数均不低于0.999 0,方法的定量限(以信噪比为10计)为0.2～0.5μg/kg,添加水平为1.0～20μg/kg时,回收率为71.5～106%,相对标准偏差(n=6)为3.2～9.1%。该法前处理简单、回收率高、精密度好,适用于水产品中7种微囊藻毒素的测定。

A new analytical method for the simultaneous determination of seven microcystins （MC-RR, MC-YtL MC-LR, MC-LA, MC-LW, MC-LF and MC-LY） in aquatic product by high performance liquid chromatography-tandem mass spectrometry （LC-MS-MS） was established. Aquatic product sample was extracted with 90% methanol （V/V）, and then the extracts were cleaned up by SPE and analyzed by LC-MS-MS using a C l8 column, employing 0.1% formic acid acetonitrile solution - 0.1% formic acid aqueous solution as the mobile phase for gradient elution. Mass spectrum was used for assistant identification. External standard method was applied for quantization. The result indicated that the limits of quantification （LOQs） of seven microcysfins were ranged from 0.2 μg/kg to 0.5 μg/kg. Meanwhile, the linear correlation coefficients （r〉 0.999 0） of seven microcystins were obtained within the irrespective linear ranges. The recoveries of seven microcystins from spiked samples at the spiking levels of 1.0-20 μg/kg were ranged from 71.5 to 106 % with RSD of 3.2 %- 9.1% （n=6）. The method was simple, precise and had high recoveries for the determination of microcystins in aquatic product samples.