分子印迹杂化介孔硅胶材料的制备及固相萃取-高效液相色谱法测定鳕鱼中氟喹诺酮类兽药残留

目的建立一种分子印迹介孔硅胶材料的制备方法,并用于鳕鱼中氟喹诺酮类药物残留的选择性富集。方法采用分子印迹技术和共缩聚法合成了苯基和氨基功能化的新型分子印迹杂化介孔硅胶材料。在最佳条件下,采用固相萃取-高效液相色谱法测定鳕鱼中氧氟沙星、洛美沙星和沙拉沙星3种氟喹诺酮类药物残留。结果在最佳固相萃取条件下,获得了较高的富集倍数(8.56)。在鱼样中,添加0.05、0.10和0.50 mg/kg的方法回收率为79.2%~95.2%,相对标准偏差为2.2%~4.9%,方法检出限(S/N=3)和定量限(S/N=10)分别为6.82~14.45?g/kg和22.73~48.45?g/kg。结论该样品处理方法选择性好、简单、快速,可用于鳕鱼中氟喹诺酮类药物残留的分离检测。

Preparation of molecularly imprinted hybrid mesoporous silica materials for determination of fluoroquinolone veterinary drug residues in codfish by solid-phase extraction-high performance liquid chromatography

Objective To establish a preparation method of molecularly imprinted mesoporous silica material for selective enrichment of fluoroquinolones drug residues in codfish. Methods A new type of molecularly imprinted hybrid mesoporous silica material based on phenyl-and amino-siloxane was synthesized by the molecular imprinting technique and co-condensation method. Under the optimal condition, the ofloxacin, lomefloxacin and sarafloxacin residues in codfish were determined by solid-phase extraction coupled with high performance liquid chromatography. Results An enrichment factor of 8.56 was obtained under optimum on-line solid phase extraction conditions. The recoveries of fluoroquinolones in fish samplesat 0.05, 0.10 and 0.50 mg/kg were in the range of 79.2%~95.2% with the relative standard deviation (RSD) of 2.2%~4.9%. The limit of detection (S/N=3) and limit of quantitation (S/N=10) of the proposed method were 6.82~14.45 mg/kg and 22.73~48.45 mg/kg, respectively. Conclusion The sample treatment method is selective, simple and rapid, which can be used for the separation and detection of fluoroquinolones in codfish samples.