分散液液微萃取-高效液相色谱法测定水中磺胺类药物残留

Development of a dispersive liquid-liquid microextraction method for the determination of sulfonamide residues in water samples by high performance liquid chromatography

建立了分散液液微萃取-高效液相色谱法测定水样中氨苯磺胺、磺胺嘧啶,磺胺二甲基嘧啶3种磺胺药物残留的检测方法。对萃取剂、分散剂的种类和体积、pH、盐浓度等影响萃取效率的因素进行了优化。在最优的萃取条件下,3种抗菌药的测定线性范围为1-1000μg/L,r≥0.9997,检出限为0.07-0.25μg/L（S/N=3）。应用于5种不同水样中磺胺类抗菌药残留的分析,目标分析物的加标回收率在82.0%-104.0%之间,相对标准偏差小于5.9%。

A novel method for the determination of sulfanilamide （ SAD）, sulfadiazine （SDZ） and sulfamethazine （ SM2 ） residues in water samples has been developed by using dispersive liquid-liquid microextraetion （DLLME） coupled with high performance liquid chromatography with DAD detection. Parameters such as type and volume of extraction solvent and disperser solvent, concentration and composition of sodium chloride and pH were optimized. The analytes were extracted under optimized pretreatment conditions. Linearity in the concentration range of 1 - 1000μg/L was obtained with regression coefficients ranging from 0. 9997 to 0. 9999 and LODs were between 0. 07 and 0. 25 μg/L. The developed method was applied to the determination of the sulfonamides in five different water samples. The spiked recoveries were from 82. 0% to 104. 0% and the relative standard deviation（RSD） was less than 5.9% （n =6）.