As extraction solvents,ionic liquids have green characteristics.In this study,an environmentally benign analytical method termed temperature-controlled ionic liquid dispersive liquid phase microextraction (TIL-DLME) c...As extraction solvents,ionic liquids have green characteristics.In this study,an environmentally benign analytical method termed temperature-controlled ionic liquid dispersive liquid phase microextraction (TIL-DLME) combined with ultra-highpressure liquid chromatography (UHPLC)-tunable ultraviolet detection (TUV) was developed for the pre-concentration and determination of triclosan (TCS),triclocarban (TCC) and methyl-triclosan (M-TCS) in water samples.Significant parameters that may affect extraction efficiencies were examined and optimized,including the types and amount of ionic liquids,volume of the diluent,heating temperature,cooling time,salt effect and pH value.Under the optimum conditions,linearity of the method was observed in the ranges of 0.0100-100 μgL-1 for TCS and M-TCS,and 0.00500-50.0 μgL-1 for TCC with correlation coefficients (r2) 】 0.9903.The limits of detection (LODs) ranged from 1.15 to 5.33 ngL-1.TCS in domestic water and TCC in reclaimed water were detected at the concentrations of 1.01 and 0.126 μgL-1,respectively.The spiked recoveries of the three target compounds in reclaimed water,irrigating water,waste water and domestic water samples were obtained in the ranges of 68.4%-71.9%,61.6%-87.8%,58.9%-74.9% and 64.9%-92.4%,respectively.Compared with the previous dispersive liquid-liquid microextraction method (DLLME) about the determination of TCS,TCC and M-TCS,this method is not only more environmentally friendly but also more sensitive.展开更多
将1-己基-3-甲基咪唑六氟磷酸([C6MIM][PF6])离子液体自聚集于磁性多壁碳纳米管(Fe3O4@MWCNTs)表面,并将其作为磁性固相吸附剂,建立了同时测定环境水样中磺胺二甲嘧啶、磺胺对甲氧嘧啶、磺胺邻二甲氧嘧啶和磺胺二甲异噁唑4种磺胺类药物...将1-己基-3-甲基咪唑六氟磷酸([C6MIM][PF6])离子液体自聚集于磁性多壁碳纳米管(Fe3O4@MWCNTs)表面,并将其作为磁性固相吸附剂,建立了同时测定环境水样中磺胺二甲嘧啶、磺胺对甲氧嘧啶、磺胺邻二甲氧嘧啶和磺胺二甲异噁唑4种磺胺类药物的涡旋辅助磁性固相萃取-高效液相色谱法。优化条件为:将20.0 mg[C6MIM][PF6]包覆的Fe3O4@MWCNTs分散于200 m L水样中,涡旋萃取15 min,磁性分离获取磁性吸附剂,3.5 m L 1.0%乙酸铵-甲醇溶液洗脱,洗脱液氮吹至干,300μL甲醇溶解后待下一步高效液相色谱/二极管阵列检测器(HPLC-PDA)分析。4种磺胺类药物在0.375~75.0μg/L范围内与峰面积呈良好的线性关系,其相关系数为0.9985~0.9996,检出限(S/N=3)为0.079~0.099μg/L,3个加标浓度水平的回收率为80.60%~99.99%,日内、日间测定的相对标准偏差分别为1.3%~6.9%和1.2%~2.9%(n=3)。结果表明,本方法简单方便,易于操作,适用于环境水样中痕量磺胺类药物的检测。展开更多
基金the support from the National High Technology Research and Development Program of China(122007AA061601)the National Natural Science Foundation of Chinathe National Basic Research Program of China(20607026,20877092& 20877005)
文摘As extraction solvents,ionic liquids have green characteristics.In this study,an environmentally benign analytical method termed temperature-controlled ionic liquid dispersive liquid phase microextraction (TIL-DLME) combined with ultra-highpressure liquid chromatography (UHPLC)-tunable ultraviolet detection (TUV) was developed for the pre-concentration and determination of triclosan (TCS),triclocarban (TCC) and methyl-triclosan (M-TCS) in water samples.Significant parameters that may affect extraction efficiencies were examined and optimized,including the types and amount of ionic liquids,volume of the diluent,heating temperature,cooling time,salt effect and pH value.Under the optimum conditions,linearity of the method was observed in the ranges of 0.0100-100 μgL-1 for TCS and M-TCS,and 0.00500-50.0 μgL-1 for TCC with correlation coefficients (r2) 】 0.9903.The limits of detection (LODs) ranged from 1.15 to 5.33 ngL-1.TCS in domestic water and TCC in reclaimed water were detected at the concentrations of 1.01 and 0.126 μgL-1,respectively.The spiked recoveries of the three target compounds in reclaimed water,irrigating water,waste water and domestic water samples were obtained in the ranges of 68.4%-71.9%,61.6%-87.8%,58.9%-74.9% and 64.9%-92.4%,respectively.Compared with the previous dispersive liquid-liquid microextraction method (DLLME) about the determination of TCS,TCC and M-TCS,this method is not only more environmentally friendly but also more sensitive.
文摘将1-己基-3-甲基咪唑六氟磷酸([C6MIM][PF6])离子液体自聚集于磁性多壁碳纳米管(Fe3O4@MWCNTs)表面,并将其作为磁性固相吸附剂,建立了同时测定环境水样中磺胺二甲嘧啶、磺胺对甲氧嘧啶、磺胺邻二甲氧嘧啶和磺胺二甲异噁唑4种磺胺类药物的涡旋辅助磁性固相萃取-高效液相色谱法。优化条件为:将20.0 mg[C6MIM][PF6]包覆的Fe3O4@MWCNTs分散于200 m L水样中,涡旋萃取15 min,磁性分离获取磁性吸附剂,3.5 m L 1.0%乙酸铵-甲醇溶液洗脱,洗脱液氮吹至干,300μL甲醇溶解后待下一步高效液相色谱/二极管阵列检测器(HPLC-PDA)分析。4种磺胺类药物在0.375~75.0μg/L范围内与峰面积呈良好的线性关系,其相关系数为0.9985~0.9996,检出限(S/N=3)为0.079~0.099μg/L,3个加标浓度水平的回收率为80.60%~99.99%,日内、日间测定的相对标准偏差分别为1.3%~6.9%和1.2%~2.9%(n=3)。结果表明,本方法简单方便,易于操作,适用于环境水样中痕量磺胺类药物的检测。
文摘将基质固相分散、离子液体均相液-液微萃取和高效液相色谱法相结合,建立一种用于肌肉组织中依诺沙星、培氟沙星、诺氟沙星和恩诺沙星4种氟喹诺酮类药物的分析方法。首先以硅胶为分散剂,以200μL 1-己基-3-甲基咪唑四氟硼酸盐([C_6mim]BF_4)离子液体为萃取剂,p H 1.0水溶液为洗脱剂,采用基质固相分散法处理样品,目标分析物被转移至洗脱液中后,再以六氟磷酸铵为离子对试剂,采用均相液-液微萃取法分离、富集目标分析物于离子液体相中,最后通过高效液相色谱-二极管阵列检测器对目标物进行定量分析。结果表明,各化合物在线性范围内具有较好的线性关系(r>0.997 4),检出限为2.9~8.6μg/kg,加标回收率在87.9%~105.3%之间,其相对标准偏差为2.2%~8.6%。本法操作简单,不使用有机溶剂,可广泛应用于动物肌肉组织中氟喹诺酮类抗生素的萃取与检测。
