MC-LR磁性分子印迹微球结合高效液相色谱-串联质谱对鱼肉中微囊藻毒素的测定

Determination of Microcystins in Fish by MC-LR Magnetic Molecular Imprinted Microspheres Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了MC-LR磁性分子印迹微球(Fe_(3)O_(4)@MIP)结合高效液相色谱串联质谱法(HPLC-MS/MS)测定鱼肉中的8种微囊藻毒素(MCs)。以MC-LR为模板,甲基丙烯酸(MAA)为功能单体,在磁性纳米颗粒外包裹SiO_(2),在其表面合成对MCs有特异性识别的MC-LR Fe_(3)O_(4)@MIP。并对其磁性、吸附性能和特异性进行检测。将MC-LR Fe_(3)O_(4)@MIP作为磁性固相萃取的吸附剂,在优化条件下测定鱼肉中8种MCs,该方法在0.1~10μg/L的范围内呈现良好的线性关系(R^(2)≥0.99),检出限均为0.05μg/kg,定量限均为0.15μg/kg,平均回收率在74.8%~92.7%之间,相对标准偏差在1.1%~4.5%之间。结果表明,利用MC-LR Fe_(3)O_(4)@MIP能实现鱼肉中MCs的绿色、高效、特异性检测。

A method of MC-LR magnetic molecularly imprinted microsphere(Fe_(3)O_(4)@MIP)combined with high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)was established to determine 8 types of microcystins(MCs)in fish.MC-LR Fe_(3)O_(4)@MIP with specific recognition for microcystins were synthesized on its surface by using MC-LR as the template,methacrylic acid as the functional monomer,and magnetic nanoparticles encapsulated in silica as the carrier.Its magnetism,adsorption performance,and specificity were tested.And it was used as an adsorbent for dispersed solid phase extraction(DSPE)to determine 8 types of MCs in fish under optimized conditions.The developed method exhibited a good linearity in the range of 0.1μg/L to 10μg/L,with correlation coefficients above 0.99.The detection limits(LODs)for all 8 types of MCs were 0.05μg/kg and the limits of quantification(LOQs)were 0.15μg/kg.The mean recoveries were within 74.8%-92.7%,with a relative standard deviation(RSD)of 1.1%-4.5%.The results indicate that using MC-LR Fe_(3)O_(4)@MIP can achieve green,efficient,and specific detection of MCs in fish.