悬浮固化液相微萃取高效液相色谱法测定环境水样中磺胺类药物

Determination of sulfonamides in environmental water samples by liquid phase microextraction based on solidification of floating organic droplet coupled with high performance liquid chromatography

建立了悬浮固化液相微萃取-高效液相色谱联用测定环境水样中磺胺类药物的方法。以正十二醇为萃取剂,利用涡旋对磺胺嘧啶、磺胺二甲嘧啶、磺胺对甲氧嘧啶进行萃取,水样体积为10 mL时的最佳萃取条件:0.8 mL正十二醇,pH 5.3,涡旋萃取60 s,以4000 r/min转速离心5 min。采用高效液相色谱外标法进行定量分析,磺胺嘧啶、磺胺二甲嘧啶、磺胺对甲氧嘧啶的质量浓度分别在3.75~60 mg/L,6.25~100 mg/L,8.75~140 mg/L范围内与色谱峰面积线性关系良好,相关系数均不小于0.9992。磺胺嘧啶、磺胺二甲嘧啶、磺胺对甲氧嘧啶的检出限分别为0.48,0.72,0.92 mg/L,定量限分别为1.59,2.40,3.05 mg/L。磺胺二甲嘧啶、磺胺对甲氧嘧啶的样品加标回收率为84.4%~87.3%,相对标准偏差分别为0.6%~2.2%(n=5)。该方法精密度和准确度均能满足磺胺二甲嘧啶、磺胺对甲氧嘧啶的检测要求。磺胺嘧啶的样品加标回收率偏低,不适于用该方法测定。

A method for the determination of sulfonamides in environmental water samples by liquid phase microextraction based on solidification of floating organic droplet coupled with high performance liquid chromatography.Dodecanol was used as an extractant to extract sulfadiazine,sulfamethazine and sulfamethoxydiazine by vortex.When the volume of water sample was 10 mL,the optimum extraction conditions were determined by optimizing the pretreatment conditions:0.8 mL n-dodecanol,pH 5.3,vortex extraction for 60 s,centrifugation speed of 4000 r/min and centrifugation time for 5 min.The external standard method of high performance loquid chromatography was used for quantitative analysis,and the concentration of three sulfonamides showed good linear with the chromatographic peak area in the ranges of 3.75-60 mg/L,6.25-100 mg/L and 8.75-140 mg/L with the correlation coefficient not less than 0.9992.The detection limits were 0.48,0.72,0.92 mg/L,and the quantitative limits were 1.59,2.40,3.05 mg/L,respectively.The average recovery of sulfamethazine and sulfamethoxydiazine was 84.4%-87.3%with the relative standard deviations of 0.6%-2.2%(n=5).The method can meet the detection requirements of sulfamethazine and sulfamethoxydiazine.The recovery of sulfadiazine was lower,which showed that the method could not suitable for the determination of sulfadiazine.