离子液体单滴微萃取-高效液相色谱法测定水体中磺胺类药物

Determination of Sulfonamides in Water Sample Using Ionic Liquid-based Single Drop Microextraction Coupled with High Performance Liquid Chromatography

应用离子液体单滴微萃取(SDME)技术,建立了水体中7种磺胺类药物的高效液相色谱(HPLC)分析方法。考察了萃取剂种类与体积、萃取时间、搅拌速度、溶液pH值、盐浓度及萃取温度对萃取效率的影响。确定了最佳萃取条件为:利用9μL1-丁基-3-甲基咪唑六氟磷酸盐([C4MIM][PF6])离子液体作为萃取液滴,在搅拌速度为300r/min、萃取温度为50℃的条件下,对pH3,NaCl浓度为0.33g/mL的10.0mL水样萃取35min。在最佳条件下,7种磺胺在0.005～2.000mg/L浓度范围内呈良好的线性关系,线性相关系数为0.9994～0.9998;检出限为0.001～0.003mg/L(S/N=3);[C4MIM][PF6]对7种磺胺的富集倍数在22～107之间;5次平行测定的相对标准偏差为3.1%～5.6%;对自来水、江水、湖水和废水的加标回收率为84.3%～106%。

A novel method was developed for the determination of seven sulfonamides in water samples using ionic liquid-based single drop microextraction coupled with high performance liquid chromatography.The influence of extraction parameters including extraction solvent,volume of extraction solvent,extraction time,stirring speed,pH value,NaCl concentration of sample solution and extraction temperature were investigated.Using 9 μL 1-butyl-3-methylimidazolium hexafluorophosphate（[C4MIM][PF6]） as extraction drop,10.0 mL aqueous sample with 0.33 g/mL NaCl（pH 3） was extracted for 35 min with stirring at 300 r/min at 50 ℃.Under the optimal conditions,good linear relationships were obtained in the sulfonamides concentrations of 0.005-2.000 mg/L with the correlation coefficients of 0.9994-0.9998;the detection limits were 0.001-0.003 mg/L（S/N = 3） ;the enrichment factors of [C4MIM][PF6]for the seven sulfonamides were from 22 to 107;the RSD of matrix spiked samples were 3.1%-5.6%（n = 5）.The proposed method was applied to the determination of the seven sulfonamides in tap,river,lake and waste water with recoveries of the seven sulfonamides in the range of 84.3%-106.0%.