Shifen Mou

Mixed hemimicelles solid-phase extraction based on cetyltrimethylammonium bromide-coated nano-magnets Fe3O4 for the determination of chlorophenols in environmental water samples coupled with liquid chromatography/spectrophotometry detection.

Mixed hemimicelles solid-phase extraction (SPE) based on cetyltrimethylammonium bromide (CTAB)-coated nano-magnets Fe3O4 was investigated for the preconcentration of four chlorophenols (CPs) in environmental water samples prior to HPLC-spectrophotometry determination in this paper. By the rapid isolating (about 5 min) of Fe3O4 nanoparticles (NPs) through placing a Nd-Fe-B strong magnet on the bottom of beaker, the time-consuming preconcentration process of loading large volume sample in conversional SPE method with a column can be avoided. The unique properties of Fe3O4 NPs such as high surface area and strong magnetism were utilized adequately in the SPE process. This novel separation method produced a high preconcentration rate and factor. A comprehensive study of the adsorption conditions such as the Fe3O4 NPs zeta-potential, CTAB added amounts, pH value, standing time and maximal extraction volume was also presented. Under optimized conditions, four analytes of 2-chlorophenol (2-CP), 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (TCP) and pentachlorophenol (PCP) were quantitatively extracted. The method was then used to determine four CPs in five real environmental water samples. High concentration factors (700) were achieved for each of the analytes, with observed detection limits ranging between 0.11 and 0.15 microg L(-1). The accuracy of method was evaluated by recovery measurements on spiked samples. Good recovery results (83-98%) with satisfactory relative standard deviation (RSD) were achieved. It is important to note that satisfactory preconcentration factors and extraction recoveries for the four CPs were obtained with only a little amount of Fe3O4 NPs (0.1g) and CTAB (60 mg). To the best of our knowledge, this was the first time a mixed hemimicelles SPE method based on Fe3O4 NPs magnetic separation had been used for the pretreatment of environmental water samples.

Determination of eight synthetic food colorants in drinks by high-performance ion chromatography.

Eight synthetic food colorants (Amaranth, Brilliant Blue, Indigo Carmine, New Red, Ponceau 4R, Sunset Yellow, Tartrazine, Allura Red) were determined by high-performance ion chromatography on an anion-exchange analytical column with very low hydrophobicity and visible absorbance detection. Gradient elution with hydrochloric acid-acetonitrile effected both the chromatographic separation of these colorants and the on-line clean-up of the analytical column, which was very advantageous for routine analysis. High-performance ion chromatography may be a solution to the chromatographic analysis for some water-soluble, organic analytes with strong hydrophobicity. The method has been applied to the determination of colorants in drinks and in instant drink powder. No time-consuming pretreatment, as used in conventional liquid chromatography, was needed.

Analysis of phthalates via HPLC-UV in environmental water samples after concentration by solid-phase extraction using ionic liquid mixed hemimicelles.

Ionic liquid mixed hemimicelles-based solid-phase extraction for the preconcentration of five phthalates in environmental water sample was investigated in this paper. A comparative study on the use of room temperature ionic liquids (RTILs) 1-hexyl-3-methylimidazolium bromide ([C(6)mim]Br) and 1-dodecyl-3-methylimidazolium bromide ([C(12)mim]Br)-coated silica as sorbents was presented. Owing to having bigger adsorption amounts for analytes [C(12)mim], Br-coated silica was selected as SPE material and the five analytes di-ethyl-phthalate (DEP), di-n-propyl-phthalate (DnPP), di-n-butyl-phthalate (DnBP), di-cyclohexyl-phthalate (DcHP) and di-(2-ethylhexyl)-phthalate (DEHP) can be quantitatively extracted under optimal conditions. The analytes retained on the cartridge were desorbed completely with 3mL methanol (pH 2). Predominant factors influencing the extraction efficiency, such as RTILs concentration, pH value, ionic strength and breakthrough volume were discussed. The proposed method had been applied to determining the five phthalates in four environmental water samples and concentration factor of 600 was achieved easily. Detection limits obtained ranged between 0.12 and 0.17mug/L. The accuracy of this method was evaluated by recovery measurement on spiked samples, and good recovery results (85-107%) with relative standard deviation (R.S.D.) of below 6% were achieved.

Direct determination of free amino acids and sugars in green tea by anion-exchange chromatography with integrated pulsed amperometric detection

Determination of amino acids and sugars in green tea by anion-exchange chromatography with integrated pulsed amperometric detection was developed. Amino acids and sugars were separated on an anion-exchange column at a flow-rate of 0.25 ml/min by using ternary gradient elution consisting of deionized water, 0.25 M sodium hydroxide, and 1.0 M sodium acetate. Under optimized conditions, theanine was separated from glutamine and three sugars (glucose, fructose, and sucrose) were eluted earlier than the neutral amino acids to avoid their interference with each other. RSDs of the peak area of analytes were lower than 4.6%. Detection limits for the analytes ranged from 0.12 to 4.9 pmol. The linearities for all analytes were two or three orders of magnitude with the correlation coefficients greater than 0.99. This method was applied to determination of amino acids and sugars in green tea with satisfactory results.

Ion chromatographic analysis of tetracyclines using polymeric column and acidic eluent.

High-performance ion chromatography (HPIC) is first successfully used to analyze tetracycline antibiotics (TCs) in this work. The TCs are well separated on a solvent compatible polymeric cation-exchange column within 12 min. Isocratic elution with acetonitrile-hydrochloride is very advantageous for routine analysis. HPIC may be seen as a specific variant of the more common high-performance liquid chromatography (HPLC) for water-soluble and polar pharmaceuticals with low hydrophobicity. The detection limits (signal-to-noise ratio=3:1) of oxytetracycline (OTC), tetracycline (TC), chlortetracycline (CTC), doxycycline (DC) are 10, 10, 20 and 20 microg l(-1), respectively. Samples are prepared by vortex mixing with an ethylenediaminetetraacetic acid disodium salt (Na2EDTA)-McIlvaine buffer (pH 4.0) solution and the mixture filtrates through a molecular weight cut-off filter. The method has been successfully applied to monitor the OTC removal rate through every reactor in the process of OTC manufacturing wastewater treatment by bio-chemical technology. It is also applicable to determine the TCs residues in milk and milk powder with satisfying results.

Separation and determination of four artificial sweeteners and citric acid by high-performance anion-exchange chromatography

Abstract A high-performance anion-exchange chromatographic method for the simultaneous separation and determination of four artificial sweeteners (sodium saccharin, aspartame, sodium cyclamate and acesulfame-K) and citric acid in a single injection is proposed. The separation was performed by an anion-exchange gradient program and determination by ultraviolet absorbance detection for sodium saccharin, aspartame, acesulfame-K in combination with conductivity detection for sodium saccharin, sodium cyclamate, acesulfame-K as well as citric acid in series. Good linearities between the concentrations of all analytes and relevant peak area responses were achieved over the range 2–100 μg/ml. The detection limits (signal-to-noise ratio 3:1) were 0.019 μg/ml for sodium saccharin, 0.035 μg/ml for aspartame, 0.044 μg/ml for acesulfame-K by ultraviolet absorbance detection and 0.26 μg/ml for sodium saccharin, 0.16 μg/ml for sodium cyclamate, 0.23 μg/ml for acesulfame-K and 0.22 μg/ml for citric acid by conductivity detection. The method has been successfully applied to the determination of the four sweeteners and citric acid in drinks and powdered tabletop sweeteners, and the average recoveries for various samples ranged from 93 to 107%.

Simultaneous determination of amino acids and carbohydrates by anion-exchange chromatography with integrated pulsed amperometric detection.

A direct, sensitive, simple and practical method for simultaneous determination of amino acids and carbohydrates by anion-exchange chromatography with integrated pulsed amperometric detection was developed. The retention behavior of amino acids and carbohydrates on the anion-exchange column and the detection of amino acids and carbohydrates at different integrated pulsed amperometric detection waveforms were investigated. The optimized gradient eluent conditions for analysis of 17 amino acids and nine carbohydrates were obtained. Separation time was 100 min. Detection limits for amino acids and carbohydrates were 5.2-207.1 nM under injection volume of 25 microl. The RSDs of peak area were 1.2-3.3%. The calibration graphs of peak area for the analytes were linear over about three orders of magnitude with a correlation coefficient of 0.9950-0.9999. The method was applied to determine amino acids and carbohydrates in a liquid condiment with satisfactory results.

Separation methods for taurine analysis in biological samples.

Taurine plays an important role in a variety of physiological functions, pharmacological actions and pathological conditions. Many methods for taurine analysis, therefore, have been reported to monitor its levels in biological samples. This review discusses the following techniques: sample preparation; separation and determination methods including high-performance liquid chromatography, gas chromatography, ion chromatography, capillary electrophoresis and hyphenation procedures. It covers articles published between 1990 and 2001.

Determination of trace level bromate and perchlorate in drinking water by ion chromatography with an evaporative preconcentration technique

A simple sample preconcentration technique employing microwave-based evaporation for the determination of trace level bromate and perchlorate in drinking water with ion chromatography is presented. With a hydrophilic anion-exchange column and a sodium hydroxide eluent in linear gradient, bromate and perchlorate can be determined in one injection within 35 min. Prior to ion chromatographic analysis, the drinking water sample was treated with an OnGuard-Ag cartridge to remove the superfluous chloride and concentrated 20-fold using a PTFE beaker in a domestic microwave oven for 15 min. The recoveries of the anions ranged from 94.6% for NO2- to 105.2% for F-. The detection limits for bromate, perchlorate, iodate and chlorate were 0.1, 0.2, 0.1 and 0.2 microg/l, respectively. The developed method is applicable for the quantitation of bromate and perchlorate in drinking water samples.

On-line pretreatment and determination of Pb, Cu and Cd at the μg l−1 level in drinking water by chelation ion chromatography

A novel, highly sensitive method for the simultaneous separation and determination of lead, copper, cadmium and other transition metals in drinking water was achieved by on-line sample pretreatment of chelation ion chromatography. Manganese, which coeluted with cadmium, was oxidized to permanganate by ammonium persulfate before injection. Permanganate, with bulk quantity of alkali, alkaline earth metals, iron and aluminum, was eliminated by pyrophosphoric acid-ammonium acetate buffer solution (pH 5.5), while retaining heavy and transition metals on a selective chelating resin (MetPac CC-1 column). Then, they were disabsorbed and transferred to a sulfonated cation exchanger (TMC-1 column). Finally, the concentrated trace metals were separated on a bifunctional ion-exchange column (CS5A) by a concentration gradient of oxalic acid and sodium nitrate eluents, coupled with post-column spectrophotometric detection with 2-[(5-bromo-2-pyridyl)azo]-5-diethylaminophenol (5-Br-PADAP) at 560 nm. The separation and color-development conditions were optimized. The detection limits for the method (signal-to-noise ratio=3:1) were at or below the mu g l(-1) level. The results of drinking water analyses were satisfactory