Zhang Qianchun, Xiao Xiaohua, Li Gongke
School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China; School of Biology and Chemistry, Xingyi Normal University for Nationalities, Xingyi 562400, China.
School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China.
Talanta. 2014 Jun;123:63-70. doi: 10.1016/j.talanta.2014.02.010. Epub 2014 Feb 12.
A novel porous molecularly imprinted monolithic capillary column (MIMCC) based on ternary porogen was synthesized by in situ technique with sulfaquinoxaline as the template molecule. The characteristics of the MIMCC were investigated by scanning electron microscopy, infrared spectrum, thermogravimetric analysis and solvent resistance test. The saturated adsorption amount of sulfaquinoxaline on MIMCC was 2.7 times over that on the non-imprinted monolithic capillary column (NIMCC). The MIMCC also exhibited good enrichment ability to its analogs and the enrichment factors were 46-211 for five antimicrobials. High permeability and imprinting factors as well as good stability, reproducibility and long lifetime were obtained. An on-line method based on MIMCC solid-phase microextraction coupled with high-performance liquid chromatography was developed for the determination of trace antimicrobials in complex samples. The good linearity for sulfametoxydiazine, sulamethoxazole and sulfaquinoxaline was 0.05-10 µg/L, the limits of detection (LODs) were 10.0-14.0 ng/L. The linear range for mequindox and quinocetone were 0.10-10.0 µg/L, the LODs were 20.0-27.0 ng/L respectively. The recoveries were 71.0-108.2% with relative standard deviation of 1.6-8.5%, correspondingly. The results showed that MIMCC could effectively enrich antimicrobials from complex matrices. The on-line method based on MIMCC and HPLC was selective, sensitive and convenient for trace determination of antimicrobials in complex samples.
以磺胺喹恶啉为模板分子，采用原位技术合成了一种基于三元致孔剂的新型多孔分子印迹整体柱（MIMCC）。通过扫描电子显微镜、红外光谱、热重分析和耐溶剂性测试对MIMCC的特性进行了研究。磺胺喹恶啉在MIMCC上的饱和吸附量是在非印迹整体柱（NIMCC）上的2.7倍。MIMCC对其类似物也表现出良好的富集能力，五种抗菌药物的富集因子为46 - 211。该整体柱具有高渗透性、印迹因子以及良好的稳定性、重现性和长使用寿命。建立了一种基于MIMCC固相微萃取与高效液相色谱联用的在线方法，用于测定复杂样品中的痕量抗菌药物。磺胺间甲氧嘧啶、磺胺甲恶唑和磺胺喹恶啉的线性良好范围为0.05 - 10 μg/L，检测限（LOD）为10.0 - 14.0 ng/L。甲喹酮和喹烯酮的线性范围为0.10 - 10.0 μg/L，LOD分别为20.0 - 27.0 ng/L。回收率为71.0 - 108.2%，相对标准偏差相应为1.6 - 8.5%。结果表明，MIMCC能够有效地从复杂基质中富集抗菌药物。基于MIMCC和HPLC的在线方法对于复杂样品中痕量抗菌药物的测定具有选择性、灵敏性和便利性。
