采用荧光柱前衍生化和整体硅胶柱分离技术测定禽肉和禽蛋提取物中磺胺类残留。

LC of sulfonamide residues in poultry muscle and eggs extracts using fluorescence pre-column derivatization and monolithic silica column.

机构信息

Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.

出版信息

J Sep Sci. 2010 Jan;33(1):11-22. doi: 10.1002/jssc.200900461.

DOI:10.1002/jssc.200900461

PMID:20024929

Abstract

A new, rapid, sensitive and selective HPLC method with fluorescence detection is described for the simultaneous determination of 12 sulfonamides, in the presence of putrescine as internal standard, after pre-column derivatization with fluorescamine. The drugs were separated on a Chromolith Performance RP-18 column (100x4.6 mm), using a gradient elution with a binary mobile phase of methanol/0.05 M acetate buffer (pH 3.4). Linearity of derivatization was obtained for concentrations from 3.0 to 300 microg/L in standard solutions. The whole procedure was evaluated and fully validated, according to the European Union Decision 2002/657/EC, for the determination of sulfonamides in turkey muscle and hen eggs following SPE. The LODs varied from 2 to 17 microg/kg in turkey and 2 to 15 microg/kg in egg samples. The average recoveries ranged between 96.9-108.6% in turkey muscle and 96.0-108.4% in egg samples, respectively.

摘要

描述了一种新的、快速、灵敏和选择性的 HPLC 方法，带有荧光检测，用于在腐胺作为内标存在的情况下，通过柱前衍生化与荧光胺同时测定 12 种磺胺类药物。药物在 Chromolith Performance RP-18 柱（100x4.6mm）上分离，使用甲醇/0.05 M 乙酸盐缓冲液（pH3.4）的二元流动相进行梯度洗脱。在标准溶液中，衍生化的线性浓度范围为 3.0 至 300μg/L。根据欧盟 2002/657/EC 号决定，对 SPE 后火鸡肉和鸡蛋中磺胺类药物的测定进行了整个程序的评估和充分验证。LOD 分别在火鸡肌肉中为 2 至 17μg/kg，在鸡蛋样品中为 2 至 15μg/kg。平均回收率分别在火鸡肌肉和鸡蛋样品中为 96.9-108.6%和 96.0-108.4%。