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盐析均匀萃取后结合离子液体/离子液体液-液微萃取用于高效液相色谱法测定血液中的磺胺类药物。

Salting-out homogenous extraction followed by ionic liquid/ionic liquid liquid-liquid micro-extraction for determination of sulfonamides in blood by high performance liquid chromatography.

作者信息

Liu Zhongling, Yu Wei, Zhang Hanqi, Gu Fanbin, Jin Xiangqun

机构信息

China-Japan Union Hospital, Jilin University, Xiantai Street 126, Changchun 130033, PR China; College of Pharmacy, Jilin University, Xinmin Street 1163, Changchun 130033, PR China.

Department of Hand Surgery, China-Japan Union Hospital, Jilin University, Xiantai Street 126, Changchun 130033, PR China.

出版信息

Talanta. 2016 Dec 1;161:748-754. doi: 10.1016/j.talanta.2016.09.006. Epub 2016 Sep 4.

Abstract

Salting-out homogenous extraction followed by ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction system was developed and applied to the extraction of sulfonamides in blood. High-performance liquid chromatography was applied to the determination of the analytes. The blood sample was centrifuged to obtain the serum. After the proteins in the serum were removed in the presence of acetonitrile, ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate, dipotassium hydrogen phosphate, ionic liquid 1-Hexyl-3-methylimidazolium hexafluorophosphate were added into the resulting solution. After the resulting mixture was ultrasonically shaken and centrifuged, the precipitate was separated. The acetonitrile was added in the precipitate and the analytes were extracted into the acetonitrile phase. The parameters affecting the extraction efficiency, such as volume of ionic liquid, amount of dipotassium hydrogen phosphate, volume of dispersant, extraction time and temperature were investigated. The limits of detection of sulfamethizole (STZ), sulfachlorpyridazine (SCP), sulfamethoxazole (SMX) and Sulfisoxazole (SSZ) were 4.78, 3.99, 5.21 and 3.77μgL, respectively. When the present method was applied to the analysis of real blood samples, the recoveries of analytes ranged from 90.0% to 113.0% and relative standard deviations were lower than 7.2%.

摘要

建立了盐析均相萃取-离子液体/离子液体分散液液微萃取体系,并将其应用于血液中磺胺类药物的萃取。采用高效液相色谱法测定分析物。将血样离心以获得血清。在乙腈存在下除去血清中的蛋白质后,向所得溶液中加入离子液体1-丁基-3-甲基咪唑四氟硼酸盐、磷酸氢二钾、离子液体1-己基-3-甲基咪唑六氟磷酸盐。将所得混合物超声振荡并离心后,分离出沉淀。向沉淀中加入乙腈,将分析物萃取到乙腈相中。研究了影响萃取效率的参数,如离子液体体积、磷酸氢二钾用量、分散剂体积、萃取时间和温度。磺胺甲噻二唑(STZ)、磺胺氯哒嗪(SCP)、磺胺甲恶唑(SMX)和磺胺异恶唑(SSZ)的检测限分别为4.78、3.99、5.21和3.77μg/L。将本法应用于实际血样分析时,分析物的回收率在90.0%至113.0%之间,相对标准偏差低于7.2%。

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