分子印迹固相萃取联用高效液相色谱分离测定海水中的膝沟藻毒素GTX1,4  

Separation and Determination of Gonyautoxins 1,4 in Seawater by Molecularly Imprinted Solid Phase Extraction Coupled with High Performance Liquid Chromatography

作　　者：梅晓颀 何秀平[1] 王江涛[1] 

机构地区：[1]中国海洋大学海洋化学理论与工程技术教育部重点实验室,青岛266100

出　　处：《分析化学》2016年第2期212-217,共6页Chinese Journal of Analytical Chemistry

摘　　要：采用分子印迹技术,以鸟嘌呤核苷为虚拟模板,本体聚合,合成GTX1,4的分子印迹聚合物(MIP)。傅里叶红外变换光谱(FT-IR)和扫描电子显微镜(SEM)的结果显示,MIP具有分布均匀、大小均一的孔穴。平衡吸附实验表明,分子印迹聚合物(MIP)比非分子印迹聚合物(NIP)具有更高的结合容量,对膝沟藻毒素GTX1,4有更好的选择性。用MIP填充固相萃取小柱(MISPE),以0.1 mol/L乙酸溶液为淋洗液,甲醇-水(95∶5,V/V)溶液为洗脱液时回收率最高,达到85.0%。用优化后的淋洗洗脱条件测定微小亚历山大藻和塔玛亚历山大藻藻液中的GTX1,4,分别为1.10和0.99μg/L,RSD分别为3.3%和4.4%,说明本方法具有较好的检测限和较高的测定精密度。A kind of molecular imprinted polymer （MIP） was synthesized by bulk polymerization using guanosine as dummy template molecule. The results of Fourier transform infrared spectrometer （FI＇-IR） and scanning electron microscope showed that MIP had homogenous and uniform-sized cavities. It was confirmed that MIP had higher binding affinity and selectivity towards gonyautoxins 1,4 （GTX1,4） than NIP according to the static equilibrium adsorption. The solid phase extraction columns were packed with MIP. The maximum recovery （85.05%） of MISPE was achieved using 0.1 mol/L acetic acid as washing solution and ethanol- water （95：5, V/V） as elution solution. Then the concentrations of GTX1,4 from culture solution of Alexandrium minutum and Alexandrium tamarense were determined to be 1.10 and 0.99 p^g/L, respectively, under the optimum conditions of washing and elution, and RSD was 3.3 % and 4.4%, respectively, indicated good LOD and higher precision.

关 键 词：膝沟藻毒素GTX1 4 分子印迹固相萃取 分离富集 微小亚历山大藻 塔玛亚历山大藻 

分 类 号：X834[环境科学与工程—环境工程] O657.72[理学—分析化学]