色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
12期
1362-1367
,共6页
吴翠琴%雷金妹%李韵灵%王韵靓%陈迪云%龚剑
吳翠琴%雷金妹%李韻靈%王韻靚%陳迪雲%龔劍
오취금%뢰금매%리운령%왕운정%진적운%공검
离子液体%分散液液微萃取%高效液相色谱%荧光检测%磺胺类药物
離子液體%分散液液微萃取%高效液相色譜%熒光檢測%磺胺類藥物
리자액체%분산액액미췌취%고효액상색보%형광검측%광알류약물
ionic liquid(IL)%dispersive liquid-liquid microextraction(DLLME)%high per-formance liquid chromatography(HPLC)%fluorescence detection%sulfonamides(SAs)
建立了一种基于离子液体的分散液液微萃取技术结合柱前荧光衍生高效液相色谱（ IL-DLLME-HPLC-FL）对8种磺胺类药物进行检测的方法，并成功应用于实际环境水样的分析。实验考察了萃取参数对磺胺萃取效率的影响及衍生产物的稳定性。最佳实验条件：以40μL[C6MIM][PF6]为萃取剂，0.1 mL 丙酮为分散剂，对 pH=4且不含 NaCl的水溶液进行不超声的分散液液微萃取，并衍生化反应6 h。结果表明：在最佳实验条件下，该法在0.2~10μg／L和10~500μg／L两个浓度范围内线性良好，线性相关系数 r ≥0.9989；检出限为0.08~0.5μg／L（ S／N=3）。对实验室自来水、湖水、珠江水、池塘水分别加标5、50、200μg／L的回收率为87.2％~101.4％，相对标准偏差为3.7％~6.2％。该法环保、简便，可用于测定实际水样中磺胺类药物。
建立瞭一種基于離子液體的分散液液微萃取技術結閤柱前熒光衍生高效液相色譜（ IL-DLLME-HPLC-FL）對8種磺胺類藥物進行檢測的方法，併成功應用于實際環境水樣的分析。實驗攷察瞭萃取參數對磺胺萃取效率的影響及衍生產物的穩定性。最佳實驗條件：以40μL[C6MIM][PF6]為萃取劑，0.1 mL 丙酮為分散劑，對 pH=4且不含 NaCl的水溶液進行不超聲的分散液液微萃取，併衍生化反應6 h。結果錶明：在最佳實驗條件下，該法在0.2~10μg／L和10~500μg／L兩箇濃度範圍內線性良好，線性相關繫數 r ≥0.9989；檢齣限為0.08~0.5μg／L（ S／N=3）。對實驗室自來水、湖水、珠江水、池塘水分彆加標5、50、200μg／L的迴收率為87.2％~101.4％，相對標準偏差為3.7％~6.2％。該法環保、簡便，可用于測定實際水樣中磺胺類藥物。
건립료일충기우리자액체적분산액액미췌취기술결합주전형광연생고효액상색보（ IL-DLLME-HPLC-FL）대8충광알류약물진행검측적방법，병성공응용우실제배경수양적분석。실험고찰료췌취삼수대광알췌취효솔적영향급연생산물적은정성。최가실험조건：이40μL[C6MIM][PF6]위췌취제，0.1 mL 병동위분산제，대 pH=4차불함 NaCl적수용액진행불초성적분산액액미췌취，병연생화반응6 h。결과표명：재최가실험조건하，해법재0.2~10μg／L화10~500μg／L량개농도범위내선성량호，선성상관계수 r ≥0.9989；검출한위0.08~0.5μg／L（ S／N=3）。대실험실자래수、호수、주강수、지당수분별가표5、50、200μg／L적회수솔위87.2％~101.4％，상대표준편차위3.7％~6.2％。해법배보、간편，가용우측정실제수양중광알류약물。
Dispersive liquid-liquid microextraction based on ionic liquid coupled with high per-formance liquid chromatography ( HPLC ) and pre-column fluorescent derivatization method ( IL-DLLME-HPLC-FL)was developed for the determination of eight sulfonamides( SAs). The influence of IL-DLLME parameters on extraction efficiency and the stability of derivatives of the eight SAs were investigated. The optimized experimental conditions were as follows:40 μL [C6MIM][PF6]as extraction solvent,0. 1 mL acetone as dispersion solvents;water sample with 0% NaCl( pH 4)was extracted by dispersive liquid-liquid microextraction without ultra-sonic-assistance and then derivatized for 6 h. Under the optimized experimental conditions,the results indicated that the eight sulfanilamides showed good linearities when their mass concen-trations were in 0. 2-10 μg/L and 10-500 μg/L,and the linear correlation coefficients were no less than 0. 998 9. The detection limits ranged from 0. 08 μg/L to 0. 5 μg/L( S/N=3). The pro-posed method was applied to the analysis of four water samples from different sources( tap water,lake water,Pearl River water and pond water ). The relative recoveries of the SAs spiked in water samples were 87. 2%-101. 4% with the relative standard deviations of 3. 7%-6. 2% at three different concentration levels of 5,50 and 200 μg/L. It is a convenient,environ-mental friendly method for the routine analysis of SAs in water samples.
