液相安培法检测鳗鱼中的磺胺类药物

Determination of sulfonamide drug residues in eels with HPLC-amperometric detection

本文建立了液相色谱安培检测鳗鱼中常用8种磺胺检测方法,采用甲醇：磷酸盐缓冲液（pH=3）梯度淋洗,反相C18分离。样品采用乙腈提取后,正己烷脱脂,用OasisMCX、MAX小柱净化后,采用玻碳电极直流安培1.3V检测。线性范围为0.05-100μg/mL,分别做3个浓度的添加回收,方法回收率在52.8～102.0%之间,方法精密度在0.8～4.6%之间,方法定量限为0.5-4μg/kg。

In this article, a method of HPLC- ED for determination of the eight commonly used sulfonamides in eels was studied. The LC separation was performed on a C18 column, with a gradient elution system of 50mol/L phosphate buffer （pH= 4） and methanol at the flow rate of 1ml/min. The sample was extracted with acetonitrile ,defated with hexane. The clean-up procedure with Oasis MCX/MAX（strong cation/anion exchange and reversed phase mixed mode） SPE column was applied in the pretreatment. The detection mode is the amperometric direct current （DC） with carbon electrode as working electrode ,and the oxidization potential 1.3V. Satisfactory linearity of eight sulfonamide was obtained in 0.05 ～ 100μg/mL. The average recovery rate range from 52.8～102.0% at three spiked level with the precision of RSD0. 8～4.6% and the quantitation limit 0.5～4μg/kg.