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Integration of solid phase extraction with HILIC-MS/MS for analysis of free amino acids in source water

Journal of Environmental Sciences 2022年第7期34卷 190-196页

作者： Junlang Qiu Caley Craven Nicholas Wawryk Kristin Carroll Xing-Fang Li Division of Analytical and Environmental Toxicology Department of Laboratory Medicine and PathologyUniversity of AlbertaEdmontonT6G 2G3Canada School of Environmental Science and Engineering Sun Yat-sen UniversityGuangzhou 510006China

Amino acids(AAs) are prevalent in source water, particularly during spring run-off. Monitoring of amino acids in source water is desirable for water treatment plants(WTP) to indicate changes in source water quality. The objective of this study was to establish analytical procedures for reliable monitoring of amino acids in source water. Therefore, we examined two different methods, large volume inject(LVI) and solid phase extraction(SPE), for sample preparation prior to HILIC-MS/MS. The LVI-HILIC-MS/MS method can provide fast and sensitive detection for clean samples, but suffers from matrix effects, resulting in irreproducible separation and shortening column lifetime. We have demonstrated that SPE was necessary prior to HILIC-MS/MS to achieve reproducible and reliable quantification of AAs in source water. A natural heterocyclic amine 1-methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid(MTCCA) was also included in the method to indicate changes in other natural nitrogenous compounds in source water. The SPE-HILIC-MS/MS method was able to achieve limits of detection from 2.6-3400 ng/L for the amino acids and MTCCA with RSDs( n = 3) of 1.1%-4.8%. As well, retention times(RT) of the analytes were reproducible with variation less than 0.01 min( n = 3) through the entire project. We further applied the SPE-HILICMS/MS method to determine AAs in authentic source water samples collected from two drinking water treatment plants(WTPs) during the 2021 spring run-off season. The results support that the SPE-HILIC-MS/MS method does not require derivatization and can provide reliable, accurate, and robust analysis of AAs and MTCCA in source water, supporting future monitoring of source water quality.

关键词： water analysis Disinfection byproducts Amino acids HPLC MS HILIC

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Derivative fluorimetry analysis of new cluster structures formed by ethanol and water molecules

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Chinese Optics Letters 2009年第2期7卷 159-161页

作者：吴斌刘莹韩彩芹骆晓森陆建倪晓武 School of Science Nanjing University of Science and Technology College of Physics and Electronic Engineering Xuzhou Normal University

The ultraviolet （UV） light excited fluorescence spectra of ethanol-water mixture with different concentrations are investigated by derivative fluorimetry. It is found that there are 8 types of luminescent cluster molecules, formed by ethanol and water molecules in different ways, existing in the solution. The peak wavelengths of all these clusters＇ fluorescence spectra are measured and their contents are obtained by measuring the peak values in the second derivative fluorescence spectra. The spectra corresponding to the 8 types of clusters are obtained by Gaussian decomposition. It is found that two kinds of cluster molecules whose peak wavelengths are 330 and 345 nm have an optimal excitation wavelength located at （236 4- 3） nm. This research contributes to the study of ethanol-water cluster structures and their physical and chemical characteristics.

关键词： Ethanol Fluorescence water analysis

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Spectrofluorimetric analysis of the Fungicide Carbendazim and Its Metabolite 2-Aminobenzimidazole in Natural water

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American Journal of Analytical Chemistry 2015年第9期6卷 767-775页

作者： Diene Diegane Thiare Abdourakhmane Khonte Amadou Diop Alphonse Mendy Atanasse Coly Francois Delattre Mame Diabou Gaye-Seye Alphonse Tine Laboratoire de Photochimie et d’Analyse(LPA) Faculte des Sciences et TechniquesUniversite Cheikh Anta DiopDakarSenegal Unite de Chimie Environnementale et Interactions sur le Vivant(UCEIV) ULCODunkerqueFrance Laboratoire de Chimie Analytique et Bromatologie(LCAB) Faculte de Medecine de Pharmacie et d’OdontologieUniversite Cheikh Anta DiopDakarSenegal

A spectrofluorimetric method for the direct analysis of carbendazim [methyl 2-benzimidazole carbamate (MBC)] fungicide and its metabolite 2-aminobenzimidazole (2-AB) in natural waters is described. Very low limit of detection (LOD) and limit of quantification (LOQ) values of 0.002 - 0.06 ng/mL and 0.006 - 0.2 ng/mL, respectively, were determined by spectrofluorimetric method with small relative standard deviation (RSD) values waters, with satisfactory recovery values of (88.5% - 119.2%).

关键词： Carbendazim 2-Aminobenzimidazole water analysis Fluorescence Analytical Method

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Study of laser-induced plasma shock waves by the probe beam deflection technique

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Chinese Optics Letters 2009年第5期7卷 410-412页

作者：钱彦陆建倪晓武 Department of Applied Physics Nanjing University of Science and Technology

Laser probe beam deflection technique is used for the analysis of laser-induced plasma shock waves in air and distilled water. The temporal and spatial variations of the parameters on shock fronts are studied as functions of focal lens position and laser energy. The influences of the characteristics of media are investigated on the well-designed experimental setup. It is found that the shock wave in distilled water attenuates to an acoustic wave faster than in air under the same laser energy. Good agreement is obtained between our experimental results and those attained with other techniques. This technique is versatile, economic, and simple to implement, being a promising diagnostic tool for pulsed laser processing.

关键词： Acoustics Laser produced plasmas Lasers Plasma shock waves Probes Thermal plumes water analysis Waves

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Study on fluorescence spectra of molecular association of acetic acid-water

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Chinese Optics Letters 2009年第4期7卷 357-360页

作者：韩彩芹刘莹杨洋倪晓武陆建骆晓森 College of Physics and Electronic Engineering Xuzhou Normal University College of Science Nanjing University of Science and Technology

Fluorescence spectra of acetic acid-water solution excited by ultraviolet （UV） light are studied, and the relationship between fluorescence spectra and molecular association of acetic acid is discussed. The results indicate that when the exciting light wavelength is longer than 246 nm, there are two fluorescence peaks located at 305 and 334 nm, respectively. By measuring the excitation spectra, the optimal wavelengths of the two fluorescence peaks are obtained, which are 258 and 284 nm, respectively. Fluorescence spectra of acetic acid-water solution change with concentrations, which is primarily attributed to changes of molecular association of acetic acid in aqueous solution. Through theoretical analysis, three variations of molecular association have been obtained in acetic acid-water solution, which are the hydrated monomers, the linear dimers, and the water separated dimers. This research can provide references to studies of molecular association of acetic acid-water, especiMly studies of hydrogen bonds.

关键词： Acetic acid Acids Dimers Fluorescence Hydrates Hydrogen Hydrogen bonds Metal analysis water analysis

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Application of Nafion/Cobalt Hexacyanoferrate Chemically Modified Electrodes for the Determination of Electroinactive Cations by Ion Chromatography

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Chinese Journal of Chemistry 2002年第8期20卷 771-776页

作者：徐继明鲜跃仲施国跃李金花金利通 Department of chemistry East China Normal University Shanghai 200062 China

An amperometric detector based on the chemical modification of Nafion and cobalt(II) hexacyanoferrate(II,III) thin film (Nafion/Co CN Fe) onto a glassy carbon (GC) electrode was firstly developed for the determination of electroinactive cations (Li +, Na +, K +, Rb +, Cs + and NH + 4) in single column ion chromatography. A set of well defined peaks of electroinactive cation was obtained. The relative standard deviations (RSDs) of chromatographic peak height (nA) for these cations were all below 3.8%. The cations were detected conveniently in the linear concentration range of 6.0×10 -6 -5.0×10 -3 mol/L and their correlation coefficients were all above 0.99. The detection limits of the cations were 9.2×10 -6 mol/L for Li +, 3.4×10 -6 mol/L for Na +, 6.3×10 -7 mol/L for K +, 7.8×10 -7 mol/L for Rb +, 6.2×10 -7 mol/L for Cs + and 6.2×10 -6 mol/L for NH + 4, at a signal noise ratio of 3. The method was quick, sensitive, simple and was successfully applied to the analysis of rainwater samples. The electrode was stable for a 2 week period of operation with no evidence of chemical or mechanical deterioration.

关键词： ion chromatography electrochemical detection water analysis

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An Electropolymerized Pyrrole-based Coating for Stir Bar Sorptive Extraction of Btex from water Followed by Gas Chromatography-Mass Spectrometry

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Chinese Journal of Chemistry 2012年第3期30卷 557-562页

作者： Babanezhad, Esmaeil Mirabi, Ali Ghodrati, Roghoieh Department of Chemistry Islamic Azad University Qaemshahr Branch Qaemshahr Iran

A stir bar sorptive extraction （SBSE） technique was developed by the use of polypyrrole （PPy） sorbent, electropolymerized on the surface of a rod, as a possible alternative to solid-phase microextraction （SPME）. Liquid desorption was subsequently employed to transfer the extracted analytes into the injection port of a gas chromatogra- phy-mass spectrometry （GC-MS）. The PPy sorbent including polypyrrole-dodecyl sulfate （PPy-DS） was deposited on the surface of a stainless steel rod from the corresponding aqueous electrolyte by applying a constant deposition potential. The developed method was applied to the trace level extraction of BTEX （benzene, toluene, ethylbenzene, o,p-xylene） from aqueous sample. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.01-0.1 ***^-1. The relative standard deviations （RSD） at a concentration level of 1 ***^-1 were obtained between 8% and 13% （n=6）. The calibration curves of BTEX showed linearity in the range of 0.03 to 600 ngomL 1. The proposed method was successfully applied to the extraction of some selected BTEX from river water samples and the relative recoveries were higher than 90% for all the analytes.

关键词： water analysis environmental analysis stir bar sorptive extraction polypyrrole BTEX GC-MS

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Determination of selected semi-volatile organic compounds in water using automated online solid-phase extraction with large-volume injection/gas chromatography/mass spectrometry

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Frontiers of Environmental Science & Engineering 2011年第3期5卷 417-425页

作者： Yongtao LI Christina L.MCCARTY Ed J.GEORGE Drinking water Quality Laboratory Underwriters Laboratories Inc.South BendIN 46617USA Chemical analysis Bruker DaltonicsFremontCA 94538USA

A rapid,sensitive,and cost-effective analyticalmethod was developed for the analysis of selected semivolatileorganic compounds in *** method used anautomated online solid-phase extraction technique coupledwith programmed-temperature vaporization large-volumeinjection gas chromatography/mass *** samples were extracted by using a fully automatedmobile rack system based on x-y-z robotic techniquesusing syringes and disposable 96-well extraction *** method was validated for the analysis of 30 semivolatileanalytes in drinking water,groundwater,andsurface *** a sample volume of 10 mL,the linearcalibrations ranged from 0.01 or 0.05 to 2.5μg·L^(-1),and themethod detection limits were less than 0.1μg·L^(-1).For thereagent water samples fortified at 1.0μg·L^(-1)and2.0μg·L^(-1),the obtained mean absolute recoveries were70%-130%with relative standard deviations of less than20%for most *** the drinking water,groundwater,and surface water samples fortified at 1.0μg·L^(-1),theobtained mean absolute recoveries were 50%-130%withrelative standard deviations of less than 20%for *** new method demonstrated three advantages:1)no manipulation except the fortification of surrogatestandards prior to extraction;2)significant cost reductionassociated with sample collection,shipping,storage,andpreparation;and 3)reduced exposure to hazardous solventsand other *** a result,this new automatedmethod can be used as an effective approach for screeningand/or compliance monitoring of selected semi-volatileorganic compounds in water.

关键词： automated solid-phase extraction programmed-temperature vaporization large-volume injection gas chromatography/mass spectrometry semi-volatile organic compounds water analysis

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Triacontyl modified silica gel as a sorbent for the preconcentration of polycyclic aromatic hydrocarbons in aqueous samples prior to gas chromatographic-mass spectrometry determination

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Chinese Chemical Letters 2010年第6期21卷 -页

作者： Tsuneaki Maeda Analytical Chemistry Division National Institute of Advanced Industrial Science and TechnologyTsukuba Central 51-1-1 HigashiTsukubaIbaraki 305-8565Japan

Triacontyl modified silica gel as a sorbent coupled with gas chromatography-mass spectrometry(GC-MS) was developed to determine EPA prior 16 polycyclic aromatic hydrocarbons(PAHs) in water *** parameters of solid-phase extraction such as organic modifier solvent,eluent,sample flow rate and volume were *** developed method was found to yield a linear calibration curve in the concentration range of 0.05-8μg/L with respect to naphthalene,acenaphthylene,acenaphthene and 0.01-8μg/L for dibenz[a,h]anthracene and 0.05-14μg/L for fluorene,phenanthrene,anthracene and 0.01-14μg/L for the rest of ***,the good accuracy and repeatability of the method made sure the requirements for achieving reliable analysis of PAHs in the environmental water samples,and the recoveries of optimal method were in the range of 80-120%except to higher volatility PAHs.C_(30)-bonded silica was proved to be an efficient sorbent for extraction of high molecular weight PAHs.

关键词： Polycyclic aromatic hydrocarbons C30-bonded silica Gas chromatography-mass spectrometry Solid-phase extraction water analysis

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Determination of Ultratrace Amounts of Copper(Ⅱ) in water Samples by Electrothermal Atomic Absorption Spectrometry After Cloud Point Extraction

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Chemical Research in Chinese Universities 2007年第2期23卷 143-147页

作者： CHEN Jian-guo CHEN neng-wu CHEN Shao-hong LIN Li ZHONG Ying-ying Department of Chemistry Xixi Campus Zhejiang University Hangzhou 310028 P. R. China Ningbo Entry-Exit Inspection and Quarantine Bureau Ningbo 315012 P. R. China

A novel approach was developed for the determination of ultratrace amounts of copper in water samples by using electrothermal atomic absorption spectrometry （ETAAS） after cloud point extraction （ CPE ）. 1-（ 2-Pyridylazo ） -2- naphthol was used as the chelating reagent and Triton X-114 as the mieellar-forming surfactant. CPE was conducted in a pH 8. 0 medium at 40 ℃ for 10 rain. After the separation of the phases by contrifugafion, the surfactant-rieh phase was diluted with 1 mL of a methanol solution of 0. 1 mol/L HNO3. Then 20μL of the diluted surfactant-rieh phase was injected into the graphite furnace for atomization in the absence of any matrix modifier. Various experimental conditions that affect the extraction and atomization processes were optimized. A detection limit of 5 ng/L was obtained after preconeentration. The linear dynamic range of the copper mass concentration was found to be 0-2.0 ng/mL, and the relative standard deviation was found to be less than 3. 1% for a sample containing 1.0 ng/mL Cu （ Ⅱ ）. This developed method was successfully applied to the determination of uhratraee amounts of Cu in drinking water, tap water, and seawater samples.

关键词： Cloud point extraction Preconeentration Electrothermal atomic absorption spectrometry Copper( Ⅱ) water analysis

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