Lijie Wu

Determination of hormones in milk by hollow fiber-based stirring extraction bar liquid-liquid microextraction gas chromatography mass spectrometry.

The hollow fiber-based stirring extraction bar liquid-liquid microextraction was applied to the extraction of hormones, including 17-α-ethinylestradiol, 17-α-estradiol, estriol, 17-β-estradiol, estrone, 17-α-hydroxyprogesterone, medroxyprogesterone, progesterone and norethisterone acetate, in milk. The present method has the advantages of both hollow fiber-liquid phase microextraction and stirring bar sorptive extraction. The stirring extraction bar was used as both the stirring bar of microextraction, and extractor of the analytes, which can make extraction, clean-up and concentration be carried out in one step. When the extraction was completed, the stirring extraction bar was easy isolated from the extraction system with the magnet. Several experimental parameters, including the type of extraction solvent, the number of hollow stirring extraction bar, extraction time, stirring speed, ionic strength, and desorption conditions were investigated and optimized. The analytes in the extract were derived and determined by gas chromatography mass spectrometry. Under optimal experimental conditions, good linearity was observed in the range of 0.20-20.00ng mL(-1). The limits of detection and quantification were in the range of 0.02-0.06ng mL(-1) and 0.07-0.19ng mL(-1), respectively. The present method was applied to the analysis of milk samples, and the recoveries of analytes were in the range of 93.6-104.6% with the relative standard deviations ranging from 1.6% to 6.2% (n=5). The results showed that the present method was a rapid and feasible method for the determination of hormones in milk samples.

Utilization of a novel microwave-assisted homogeneous ionic liquid microextraction method for the determination of Sudan dyes in red wines.

A novel microwave-assisted homogeneous ionic liquid microextraction (MA-HILME) method was first developed for the extraction of Sudan dyes in red wines followed by detection using high-performance liquid chromatography. 1-dodecyl-3-methylimidazolium bromide ([C12MIM]Br) was used as extractant in a microwave-assisted extraction (MAE) procedure, and then transferred into hydrophobic solid-state ionic liquid after adding ammonium hexafluorophosphate ([NH4][PF6]). The separation between liquid state sample and solid state extractant can be realized easily. Several experimental parameters, including type and amount of extraction solvent, microwave power and irradiation time, amount of ion-exchange reagent ([NH4][PF6]), pH of sample solution, and ionic strength, were evaluated. Under the optimum experimental conditions, the linearity for the determining of the analytes was in the range of 0.5-100 μg L(-1), with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for Sudan I, Sudan II, Sudan III, and Sudan IV were 0.19, 0.18, 0.24, and 0.16 μg L(-1), respectively. When the present method was applied to the determination of Sudan dyes in red wines, satisfactory recoveries were obtained in the range of 78.5-106.8%, and relative standard deviations were lower than 9.7%.

Ionic liquid‐based microwave‐assisted surfactant‐improved dispersive liquid–liquid microextraction and derivatization of aminoglycosides in milk samples

A green and simple method, ionic liquid-based microwave-assisted surfactant-improved dispersive liquid-liquid microextraction and derivatization was developed for the determination of aminoglycosides in milk samples. Nonionic surfactant Triton X-100 and ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate were used as the disperser and extraction solvent, respectively. Extraction, preconcentration, and derivatization of aminoglycosides were carried out in a single step. Several experimental parameters, including type and volume of extraction solvent, type and concentration of surfactant, microwave power and irradiation time, concentration of derivatization reagent, and pH value and volume of buffer were investigated and optimized. Under the optimum experimental conditions, the linearities for determining the analytes were in the range 0.4-10.0 ng/mL for tobramycin, 1.0-25.0 ng/mL for neomycin, and 2.0-50.0 ng/mL for gentamicin, with the correlation coefficients ranging from 0.9991 to 0.9998. The LODs for the analytes were between 0.11 and 0.50 ng/mL. The present method was applied to the analysis of different milk samples, and the recoveries of aminoglycosides obtained were in the range 96.4-105.4% with the RSDs lower than 5.5%. The results showed that the present method was a rapid, convenient, and environmentally friendly method for the determination of aminoglycosides in milk samples.

Application of magnetic solvent bar liquid-phase microextraction for determination of organophosphorus pesticides in fruit juice samples by gas chromatography mass spectrometry.

A simple, rapid and sensitive sample pretreatment technique, magnetic solvent bar liquid-phase microextraction (MSB-LPME) was developed for extracting organophosphorus pesticides from fruit juice. The analytes were extracted from the sample to the organic solvent immobilized in the fiber. The magnetic solvent bar not only can be used to stir the samples but also extract the analytes. After extraction, the analyte-adsorbed magnetic solvent bar can be readily isolated from the sample solution by a magnet, which could greatly simplify the operation and reduce the whole pretreatment time. The bar was eluted with methanol. The elute was evaporated to dryness and residue was dissolved in hexane. Several experimental parameters were investigated and optimized, including type of extraction solvent, number of magnetic solvent bar, extraction temperature, extraction time, salt concentration, stirring speed, pH and desorption conditions. The recoveries were in the range of 81.3-104.6%, and good reproducibilities were obtained with relative standard deviation below 6.1%.

An absorbing microwave micro-solid-phase extraction device used in non-polar solvent microwave-assisted extraction for the determination of organophosphorus pesticides.

A single-step extraction-cleanup method, including microwave-assisted extraction (MAE) and micro-solid-phase extraction (μ-SPE), was developed for the extraction of ten organophosphorus pesticides in vegetable and fruit samples. Without adding any polar solvent, only one kind of non-polar solvent (hexane) was used as extraction solvent in the whole extraction step. Absorbing microwave μ-SPE device, was prepared by packing activated carbon with microporous polypropylene membrane envelope, and used as not only the sorbent in μ-SPE, but also the microwave absorption medium. Some experimental parameters effecting on extraction efficiency was investigated and optimized. 1.0 g of sample, 8 mL of hexane and three absorbing microwave μ-SPE devices were added in the microwave extraction vessel, the extraction was carried out under 400 W irradiation power at 60°C for 10 min. The extracts obtained by MAE-μ-SPE were directly analyzed by GC-MS without any clean-up process. The recoveries were in the range of 93.5-104.6%, and the relative standard deviations were lower than 8.7%.

Dynamic microwave-assisted extraction combined with continuous-flow microextraction for determination of pesticides in vegetables

A simple, rapid, solventless and cost-effective dynamic microwave-assisted extraction (DMAE) combined with continuous-flow microextraction (CFME) system was firstly assembled and validated for extraction of eight organophosphorus pesticides in vegetables. The method combines the advantages of DMAE and CFME, and extends the application of the single drop microextraction to complex solid samples. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, analytes were first extracted from the vegetables using 3% NaCl solution as extraction solvent, then concentrated into microextraction solvent. After extraction, the microextraction solvent containing the enriched analyte was directly analyzed by GC-MS without any filtration or clean-up process. Several parameters affecting the extraction efficiency were investigated and optimized. Real vegetable samples were analyzed, satisfactory recoveries were obtained in the range of 80.7-106.7%, and relative standard deviations were lower than 8.7%.

Dynamic microwave assisted extraction coupled with dispersive micro-solid-phase extraction of herbicides in soybeans.

Non-polar solvent dynamic microwave assisted extraction was firstly applied to the treatment of high-fat soybean samples. In the dispersive micro-solid-phase extraction (D-µ-SPE), the herbicides in the high-fat extract were directly adsorbed on metal-organic frameworks MIL-101(Cr). The effects of several experimental parameters, including extraction solvent, microwave absorption medium, microwave power, volume and flow rate of extraction solvent, amount of MIL-101(Cr), and D-µ-SPE time, were investigated. At the optimal conditions, the limits of detection for the herbicides ranged from 1.56 to 2.00 μg kg(-1). The relative recoveries of the herbicides were in the range of 91.1-106.7%, and relative standard deviations were equal to or lower than 6.7%. The present method was simple, rapid and effective. A large amount of fat was also removed. This method was demonstrated to be suitable for treatment of high-fat samples.

Medium-assisted non-polar solvent dynamic microwave extraction for determination of organophosphorus pesticides in cereals using gas chromatography-mass spectrometry.

A fast and green pretreatment method, medium-assisted non-polar solvent dynamic microwave extraction, was first applied to extract ten of organophosphorus pesticides (OPPs) from five cereal samples. Without adding any polar solvent, graphite powders (GP) were used as microwave absorption medium to transform microwave energy into heat energy. For recycling GP, an extractor was made by sealing GP inside the exterior tube of a glass sleeve. By dynamic microwave extraction using hexane as extraction solvent, ten OPPs could be extracted completely within 200s, and the extract was directly analysed by GC-MS without any clean-up process. The effects of some experimental parameters on extraction efficiency were investigated and optimised. Relative standard deviations of intra- and inter-day ranging from 1.02% to 5.32% were obtained. Five real samples were analysed, and the recoveries obtained were in the range of 73.2-99.8%, and the relative standard deviations were lower than 6.63%.

Dynamic microwave-assisted extraction online coupled with single drop microextraction of organophosphorus pesticides in tea samples

A new method for the determination of seven organophosphorus pesticides was developed using dynamic microwave-assisted extraction online coupled with single drop microextraction prior to gas chromatographic mass spectrometry (GC-MS). The method combines the advantages of dynamic microwave-assisted extraction and single-drop microextraction, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, tea samples were extracted with 25% ethanol aqueous solution and purified with acidic alumina at the same time, and then the analytes were concentrated into microextraction solvent. When the extraction was completed, the solvent microdrop containing the enriched analytes was retracted into the microsyringe and directly analyzed by GC-MS without any filtration or cleanup step. The method makes extraction, cleanup, separation, and enrichment to be carried out in one step. Several experimental parameters, including type of extraction solvent, type and amount of dispersant, type and volume of microextraction solvent, microwave power, extraction time, and flow rate of extraction solvent were investigated and optimized. Under optimal experimental conditions, good linearity was observed in the range of 2.00-500.00 μg kg(-1). The limits of detection and quantification were in the range of 0.4-1.7 μg kg(-1) and 1.1-5.6 μg kg(-1), respectively. The present method was applied to the analysis of tea samples, and the recoveries of analytes were in the range of 84.9-106.4% with the relative standard deviations ranging from 1.0 to 6.1%. The results showed that the present method was a rapid and feasible method for the determination of organophosphorus pesticides in tea samples.

Ionic-liquid-impregnated resin for the microwave-assisted solid–liquid extraction of triazine herbicides in honey

Microwave-assisted ionic-liquid-impregnated resin solid-liquid extraction was developed for the extraction of triazine herbicides, including cyanazine, metribuzin, desmetryn, secbumeton, terbumeton, terbuthylazine, dimethametryn, and dipropetryn in honey samples. The ionic-liquid-impregnated resin was prepared by immobilizing 1-hexyl-3-methylimidazolium hexafluorophosphate in the microspores of resin. The resin was used as the extraction adsorbent. The extraction and enrichment of analytes were performed in a single step. The extraction time can be shortened greatly with the help of microwave. The effects of experimental parameters including type of resin, type of ionic liquid, mass ratio of resin to ionic liquid, extraction time, amount of the impregnated resin, extraction temperature, salt concentration, and desorption conditions on the extraction efficiency, were investigated. A Box-Behnken design was applied to the selection of the experimental parameters. The recoveries were in the range of 80.1 to 103.4% and the relative standard deviations were lower than 6.8%. The present method was applied to the analysis of honey samples.