Trace determination of hexabromocyclododecane diastereomers in water samples with temperature controlled ionic liquid dispersive liquid phase microextraction

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.

Simultaneous determination of free methamphetamine,pethidine,ketamine and tramadol in urine by dispersive liquid–liquid microextraction combined with GC–MS

A simple and rapid dispersive liquid–liquid microextraction(DLLME)technique coupled with gas chromatography–ion trap mass spectrometry(GC–MS)was developed for the extraction and analysis of methamphetamine(MA),pethidine(PD),ketamine(KT)and tramadol(TD)from human urine.In this study,different parameters affecting the extraction process such as the type and volume of extraction solvent,type and volume of disperser solvent,extraction time and pH value and salt effect were studied and optimized.Under optimized conditions,the enrichment factor ranged from 185 to 226 and the average recovery ranged from 80.45%to 95.55%.The linear range was 10.0–1000.0 mg/L,the limit of detection and quantitation were in the range 0.43–1.96 mg/L and 1.44–6.53 mg/L,respectively.The relative standard deviations were in the range 1.98%–3.90%(n=7).The obtained results show that DLLME combined with GC–MS is a fast and simple method for the determination of MA,PD,KT and TD in human urine.

Combination of ionic liquid dispersive liquid-phase microextraction and high performance liquid chromatography for the determination of triazine herbicides in water samples

A temperature-controlled ionic liquid dispersive liquid-phase microextraction in combination with high performance liquid chromatography was developed for the enrichment and determination of triazine herbicides such as cyanazine,simazine,and atrazine in water samples.1-Octyl-3-methylimidazolium hexafluorophosphate（[C8MIM][PF6]） was selected as the extraction solvent.Several experimental parameters were optimized.Under the optimal conditions,the linear range for cyanazine was in the concentration range of 0.5–80 mg/L and the linear range for simazine and atrazine was in the range of1.0–100 mg/L.The limit of detection（LOD,S/N = 3） was in the ranges of 0.05–0.06 mg/L,and the intra day and inter day precision（RSDs,n = 6） was in the ranges of 3.2%–6.6% and 4.8%–8.9%,respectively.Four real water samples were analyzed with the developed method,and the experimental results showed that the spiked recoveries were satisfactory.All these exhibited that the developed method was a valuable tool for monitoring such pollutants.

Dispersive liquid–liquid microextraction of silver nanoparticles in water using ionic liquid1-octyl-3-methylimidazolium hexafluorophosphate

Using the ionic liquid（IL）1-octyl-3-methylimidazolium hexafluorophosphate as the extractant and methanol as the dispersion solvent,a dispersive liquid–liquid microextraction method was developed to extract silver nanoparticles（AgN Ps）from environmental water samples.Parameters that influenced the extraction efficiency such as IL concentration,pH and extraction time were optimized.Under the optimized conditions,the highest extraction efficiency for AgN Ps was above 90% with an enrichment factor of 〉90.The extracted AgN Ps in the IL phase were identified by transmission electron microscopy and ultraviolet–visible spectroscopy,and quantified by inductively coupled plasma mass spectrometry after microwave digestion,with a detection limit of 0.01 μg/L.The spiked recovery of AgN Ps was 84.4% with a relative standard deviation（RSD）of 3.8%（n = 6）at a spiked level of 5 μg/L,and 89.7% with a RSD of 2.2%（n = 6）at a spiked level of 300 μg/L,respectively.Commonly existed environmental ions had a very limited influence on the extraction efficiency.The developed method was successfully applied to the analysis of Ag NPs in river water,lake water,and the influent and effluent of a wastewater treatment plant,with recoveries in the range of 71.0%–90.9% at spiking levels of 0.11–4.7 μg/L.