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超声辅助离子液体/离子液体分散液液微萃取-高效液相色谱法测定婴幼儿配方奶粉中的磺胺类药物

Ultrasound-assisted ionic liquid/ionic liquid-dispersive liquid-liquid microextraction for the determination of sulfonamides in infant formula milk powder using high-performance liquid chromatography.

机构信息

College of Chemistry, Jilin University, Qianjin Street 2699, Changchun 130012, PR China.

出版信息

Talanta. 2012 Sep 15;99:875-82. doi: 10.1016/j.talanta.2012.07.050. Epub 2012 Jul 24.

Abstract

Ultrasound-assisted ionic liquid/ionic liquid-dispersive liquid-liquid microextraction (UA-IL/IL-DLLME) high-performance liquid chromatography was developed and applied to the extraction, separation and determination of sulfonamides in infant formula milk powder samples. The hydrophobic IL and hydrophilic IL were used as extraction solvent and dispersion solvent, respectively. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of [C(6)MIM][PF(6)] dispersed entirely into sample solution with help of [C(4)MIM][BF(4)]. The purification of sample and concentration of target analytes were performed simultaneously. The introduction of ion-pairing agent (NH(4)PF(6)) was beneficial to the improvement of recoveries for IL phase and analytes. The experimental parameters of the UA-IL/IL-DLLME, including concentration of [C(6)MIM][PF(6)] and [C(4)MIM][BF(4)] in sample solution, ultrasound extraction time, pH value of sample solution and amount of ion-pairing agent (NH(4)PF(6)), were evaluated. The limits of detection for sulfamerazine, sulfamethizole, sulfachlorpyridazine, sulfamonomethoxine, sulfmethoxazole and sulfisoxazole were 2.94, 9.26, 16.7, 5.28, 3.35 and 6.66 μg kg(-1), respectively. When the present method was applied to the analysis of infant formula milk powder samples, the recoveries of the analytes ranged from 90.4% to 114.8% and relative standard deviations were lower than 7.5%. The proposed method was compared with the ionic liquid-homogeneous liquid-liquid microextraction, ionic liquid-ultrasound-assisted emulsification-microextraction and ionic liquid-temperature-controlled-DLLME. The results indicated that the proposed method is effective for the extraction of the sulfonamides in milk powder samples.

摘要

超声辅助离子液体/离子液体分散液液微萃取(UA-IL/IL-DLLME)高效液相色谱法被开发并应用于婴儿配方奶粉样品中磺胺类药物的提取、分离和测定。疏水性 IL 和亲水性 IL 分别用作萃取溶剂和分散溶剂。萃取过程是由浊液的形成诱导的,浊液由[C(6)MIM][PF(6)]的细微液滴完全分散在样品溶液中形成,这得益于[C(4)MIM][BF(4)]的帮助。同时进行样品的净化和目标分析物的浓缩。引入离子对试剂(NH(4)PF(6))有利于提高 IL 相和分析物的回收率。超声辅助离子液体/离子液体分散液液微萃取的实验参数,包括样品溶液中[C(6)MIM][PF(6)]和[C(4)MIM][BF(4)]的浓度、超声萃取时间、样品溶液的 pH 值和离子对试剂(NH(4)PF(6))的用量,都进行了评估。磺胺嘧啶、磺胺甲噁唑、磺胺氯哒嗪、磺胺甲噁二甲氧嘧啶、磺胺甲氧哒嗪和磺胺异噁唑的检测限分别为 2.94、9.26、16.7、5.28、3.35 和 6.66μg kg(-1)。当本方法应用于婴儿配方奶粉样品分析时,分析物的回收率在 90.4%至 114.8%之间,相对标准偏差低于 7.5%。该方法与离子液体均相液液微萃取、离子液体超声辅助乳化微萃取和离子液体温度控制 DLLME 进行了比较。结果表明,该方法对于奶粉样品中磺胺类药物的提取是有效的。

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