分析测试学报Issue(10):1148-1153,6.DOI:10.3969/j.issn.1004-4957.2014.10.009
基于涡流色谱技术的在线固相萃取/高效液相色谱-荧光检测法结合在线稀释快速测定牛奶中5种氟喹诺酮抗生素残留
Rapid Determination of Five Fluoroquinolones Antibiotic Residues in Milk by Turboflow Chromatography-based Online SPE/HPLC-Fluorescence Detection Combined with Online-dilution
张艳海 1金燕1
作者信息
- 1. 赛默飞世尔科技 中国 有限公司,上海 201205
- 折叠
摘要
Abstract
A rapid method was established for determination of five fluoroquinolones antibiotic resi-dues in milk. Sample solution was injected after protein precipitating with 0. 2% trichloroacetic acid-acetonitrile(90 : 10). Turboflow column was used as SPE column to enrich sample through large volume injection and cleanup with left pump of dual gradient LC. Strong solvent stored in 100 micro-liter loop was used to transfer the analyte which was diluted with right pump of DGLC in online mode. Then peak shape and resolution were improved by peak refocusing effect. The limits of detection ( LODs)were between 0. 01 μg/L and 0. 13 μg/L by fluorescence detection,which were far below the maximum residue levels for milk set by the EU regulations. The linearity of this method was good in the certain concentration range. The mean recoveries were in the range of 75. 9% - 95. 7% . The results indicated that this method is simple,rapid and sensitive,and is suitable for the determination of five fluoroquinolones antibiotic residues in milk.关键词
涡流色谱/在线固相萃取/液相色谱/氟喹诺酮/牛奶/在线稀释/兽药残留Key words
turbulent flow chromatography/online SPE/liquid chromatography/fluoroquinolones/milk/online dilution/veterinary residue分类
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张艳海,金燕..基于涡流色谱技术的在线固相萃取/高效液相色谱-荧光检测法结合在线稀释快速测定牛奶中5种氟喹诺酮抗生素残留[J].分析测试学报,2014,(10):1148-1153,6.