限进材料固相萃取-高效液相色谱在线联用检测牛奶中四环素类抗生素残留  

Determination of Tetracycline Residues in Milk by On-line Coupling of Restricted Access Material Solid Phase Extraction with High Performance Liquid Chromatography

作　　者：杨旭[1] 刘美娇[1] 林深[1] 徐丹[1] 董襄朝[1] 

机构地区：[1]南开大学化学学院,天津300071

出　　处：《分析化学》2016年第1期146-151,共6页Chinese Journal of Analytical Chemistry

摘　　要：建立了一种限进材料固相萃取-高效液相色谱在线联用检测牛奶中四环素类抗生素残留的分析方法。利用原子转移自由基聚合法制备的限进型聚（苯乙烯-co-二乙烯苯）键合硅胶作为同时富集四环素类小分子和排阻蛋白大分子的固相萃取材料。经过限进萃取柱的净化和富集后,牛奶样品中的四环素类抗生素（土霉素、四环素和金霉素）被反冲进反相C18分析柱进行色谱分离和测定。牛血清蛋白在限进萃取柱上的洗脱率为96.0%,说明制备的限进材料具有很好的排阻大分子蛋白的效果。3种四环素类抗生素在牛奶样品中的加标回收率为88.3%-101.5%,RSD〈8.0%;方法检出限为50-80μg/L,线性范围为0.05-2.0μg/mL。结果表明,本方法简单高效,淮确度好,检出限达到了规定要求,可以作为检测牛奶样品中四环素类抗生素残留的方法。A new method has been developed for the determination of tetracycline residues in milk by on-line restricted access material solid phase extraction-HPLC analysis.Restricted accessed poly（styrene-codivinylbenzene） bonded silica,synthesized by atom transfer radical polymerization,was used as solid phase extraction material in the experiment.This material played both functions of tetracylines extraction and biomacromolecule exclusion.Tetracyclines extracted from milk sample were back-flushed into a reversed phase C18 analytical column and oxytetracycline,tetracycline and chlortetracycline were separated and quantified by HPLC analysis.The exclusion ratio of bovine serum albumin from the restricted access material column was96.0%,which indicated that the restricted access material had the ability to exclude large biological molecules.The recoveries of three tetracylines in milk samples were 88.3%-101.5%with relative standard deviations 〈8.0%.The detection limits of 50-80 μg/L and the linear ranges from 0.05 μg/mL to2.0 μg/mL for the analytes were obtained.The results demonstrated that the method could be used in the determination of tetracycline residues in milk samples with good sensitivity and efficiency.

关 键 词：限进型聚(苯乙烯-co-二乙烯苯)键合硅胶 固相萃取-高效液相色谱在线联用 四环素类抗生素 牛奶 

分 类 号：O657.72[理学—分析化学]