A novel temperature controlled ionic liquid dispersive liquid phase microextracfion （TCIL-DLPME） coupled with rapid resolution liquid chromatography-electrospray tandem mass spectrometry （RRLC-ESI-MS-MS） has been ...A novel temperature controlled ionic liquid dispersive liquid phase microextracfion （TCIL-DLPME） coupled with rapid resolution liquid chromatography-electrospray tandem mass spectrometry （RRLC-ESI-MS-MS） has been developed for the enrichment and determination of three hexabromocyclododecane diastereomers （HBCDs） in water samples. Green solvent ionic liquid （IL） was used as extraction solvent instead of toxic organic solvents. This technique also avoided the usage of dispersive solvent. Some important parameters that might affect the extraction efficiency were optimized. Under the optimum conditions, good linear relationship, sensitivity and reproducibility were obtained. All the limits of detection for the three diastereomers were 0.1 ng/ mL. The linear range was obtained in the range of 1-100 ng/mL for the total amount of three HBCD diastereomers. It was satisfactory to analyze real environmental water samples with the recoveries ranging from 77.2% to 99.3%. The main advantage of the method is toxic organic solvent-free.展开更多
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)com...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 0.0100-100μgL-1 for TCS and M-TCS,and 0.00500-50.0μgL-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 0.126μgL-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
基金financially supported by National Water Pollution Control and Management Technology Major Projects(No.2009ZX07210-009)Scientific and Technological Developing Project of Shandong Province(No. 2009GG20001021-9)+1 种基金Open Research Fund Program of Shandong Provincial Key Laboratory of Eco-Environmental Science for Yellow River Delta(No.2009KFJJ01)Basic Foundation of Shandong Academy of Sciences and Analysis and Test center of Shandong province
文摘A novel temperature controlled ionic liquid dispersive liquid phase microextracfion （TCIL-DLPME） coupled with rapid resolution liquid chromatography-electrospray tandem mass spectrometry （RRLC-ESI-MS-MS） has been developed for the enrichment and determination of three hexabromocyclododecane diastereomers （HBCDs） in water samples. Green solvent ionic liquid （IL） was used as extraction solvent instead of toxic organic solvents. This technique also avoided the usage of dispersive solvent. Some important parameters that might affect the extraction efficiency were optimized. Under the optimum conditions, good linear relationship, sensitivity and reproducibility were obtained. All the limits of detection for the three diastereomers were 0.1 ng/ mL. The linear range was obtained in the range of 1-100 ng/mL for the total amount of three HBCD diastereomers. It was satisfactory to analyze real environmental water samples with the recoveries ranging from 77.2% to 99.3%. The main advantage of the method is toxic organic solvent-free.
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 0.0100-100μgL-1 for TCS and M-TCS,and 0.00500-50.0μgL-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 0.126μgL-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.
