Tao Yong, Liu Jing-Fu, Hu Xia-Lin, Li Hong-Cheng, Wang Thanh, Jiang Gui-Bin
School of Earth and Space Sciences, University of Science and Technology of China, Hefei 230026, China.
J Chromatogr A. 2009 Aug 28;1216(35):6259-66. doi: 10.1016/j.chroma.2009.06.025. Epub 2009 Jun 11.
By using ionic liquid as membrane liquid and tri-n-octylphosphine oxide (TOPO) as additive, hollow fiber supported liquid phase microextraction (HF-LPME) was developed for the determination of five sulfonamides in environmental water samples by high-performance liquid chromatography with ultraviolet detection The extraction solvent and the parameters affecting the extraction enrichment factor such as the type and amount of carrier, pH and volume ratio of donor phase and acceptor phase, extraction time, salt-out effect and matrix effect were optimized. Under the optimal extraction conditions (organic liquid membrane phase: [C(8)MIM][PF(6)] with 14% TOPO (w/v); donor phase: 4mL, pH 4.5 KH(2)PO(4) with 2M Na(2)SO(4); acceptor phase: 25microL, pH 13 NaOH; extraction time: 8 h), low detection limits (0.1-0.4microg/L, RSD<or=5%) and good linear range (1-2000ng/mL, R(2)>or=0.999) were obtained for all the analytes. The presence of humic acid (0-25mg/L dissolved organic carbon) and bovine serum albumin (0-100microg/mL) had no significant effect on the extraction efficiency. Good spike recoveries over the range of 82.2-103.2% were obtained when applying the proposed method on five real environmental water samples. These results indicated that this present method was very sensitive and reliable with good repeatabilities and excellent clean-up in water samples. The proposed method confirmed hollow fiber supported ionic liquid membrane based LPME to be robust to monitoring trace levels of sulfadiazine, sulfamerazine, sulfamethazine, sulfadimethoxine and sulfamethoxazole in aqueous samples.
以离子液体为膜液,三正辛基氧化膦(TOPO)为添加剂,建立了中空纤维支撑液膜微萃取(HF-LPME)结合高效液相色谱-紫外检测法测定环境水样中5种磺胺类药物的方法。对萃取溶剂以及影响萃取富集因子的参数,如载体的类型和用量、供体相和受体相的pH值及体积比、萃取时间、盐析效应和基质效应等进行了优化。在最佳萃取条件下(有机液膜相:含14% TOPO(w/v)的[C(8)MIM][PF(6)];供体相:4mL,pH 4.5的KH(2)PO(4) 与2M Na(2)SO(4);受体相:25μL,pH 13的NaOH;萃取时间:8 h),所有分析物均获得了低检测限(0.1 - 0.4μg/L,RSD≤5%)和良好的线性范围(1 - 2000ng/mL,R(2)≥0.999)。腐殖酸(0 - 25mg/L溶解有机碳)和牛血清白蛋白(0 - 100μg/mL)的存在对萃取效率无显著影响。将该方法应用于5种实际环境水样时,加标回收率在82.2% - 103.2%范围内。这些结果表明,该方法灵敏度高、可靠,具有良好的重复性和出色的水样净化效果。所提出的方法证实了中空纤维支撑离子液体膜基液膜微萃取在监测水样中痕量磺胺嘧啶、磺胺甲嘧啶、磺胺二甲嘧啶、磺胺二甲氧嘧啶和磺胺甲恶唑方面具有稳健性。