Over recent decades, Gampaha district, Sri Lanka, has experienced significant urbanisation and industrial growth, increasing groundwater demand due to limited and polluted surface water resources. In 2013, a community...Over recent decades, Gampaha district, Sri Lanka, has experienced significant urbanisation and industrial growth, increasing groundwater demand due to limited and polluted surface water resources. In 2013, a community uprising in Rathupaswala, a village in Gampaha district, accused a latex glove manufacturing factory of causing groundwater acidity (pH < 4). This study evaluates the spatial and temporal changes in geochemical parameters across three transects in the southern part of Gampaha district to 1) assess the impact of geological formations on groundwater;2) compare temporal variations in groundwater;and 3) explain acidification via a geochemical model. Seventy-two sample locations were tested for pH, electrical conductivity (EC), and anion concentrations (sulphate, nitrate, chloride and fluoride). Depth to the water table and distance from the sea were measured to study variations across sandy, peaty, lateritic, and crystalline aquifers. Results showed pH readings around 7 for sandy and crystalline aquifers, below 7 for peaty aquifers, and below 5 for lateritic aquifers, with significant water table fluctuations near Rathupaswala area. Principal component analysis revealed three principal components (PCs) explaining 86.0% of the variance. PC1 (40.6%) correlated with pH, EC, and sulphate (saltwater intrusion), while PC2 (32.0%) correlated with nitrates and depth to the water table (anthropogenic nutrient pollution). A geochemical transport model indicated a cone of depression recharged by acidic groundwater from peat-soil aquifers, leading to acidic groundwater in Rathupaswala area. Previous attributions of acidic pH to the over-exploitation of groundwater by the latex factory have been reevaluated;the results suggest natural acidification from prolonged water-rock interactions with iron-rich lateritic aquifers. Groundwater pH is influenced by local climate, geology, topography, and drainage systems. It is recommended that similar water-rock interaction conditions may be present throughout the wet zone of Sri Lanka, warranting detailed studies to confirm this hypothesis.展开更多
[Objective] The aim was to analyze sugar components in fermented rice wine by ion chromatography. [Method] The optimal condition for chromatography system of sugar analysis was selected by measuring sugars in fermente...[Objective] The aim was to analyze sugar components in fermented rice wine by ion chromatography. [Method] The optimal condition for chromatography system of sugar analysis was selected by measuring sugars in fermented rice wine with ion chromatography and pulsed amperometric detection. [Result] The optimal measurement conditions were as follows: Leacheate (Leachate), consisting of NaOH and CH3COONa, was eluted by gradient concentrations, with column temperature at 35 ℃ and flow rate at 0.4 ml/min. In the condition, sugars in rice wine were ana- lyzed and the results showed that the method is featured by low detection limit, good repetition and high recovery rate. [Conclusion] The research establishes and determines the approaches and optimum conditions for sugar analysis in rice wine by ion chromatography and pulsed amperometric detection, providing references for advancement of research on quality improvement of fermented rice wine.展开更多
The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hosp...The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples' turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.展开更多
A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F -, Cl -, NO - 2, NO - 3, SO 2- 3, SO 2- ...A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F -, Cl -, NO - 2, NO - 3, SO 2- 3, SO 2- 4, PO 3- 4), and fifteen water-soluble organic ions(formate, acetate, MSA, oxalate, malonate, succinate, phthalates, etc.) in atmospheric aerosols. The linear concentrations ranged from 0.005 μg/m 3 to 500 μg/m 3(r = 0.999—0.9999). The relative standard deviation(RSD) were 0.43%—2.00% and the detection limits were from 2.7 ng/m 3 to 88 ng/m 3. The proposed method was successfully applied to the simultaneous determination of those inorganic ions and organic ions in PM 2.5 of Beijing.展开更多
With the expansion of herbal medicine (HM) market, the issue on how to apply up-to- date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention...With the expansion of herbal medicine (HM) market, the issue on how to apply up-to- date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention. Due to its inherent characteristics of accurate mass measurements and multiple stages analysis, the integrated strategy of liquid chromatography (LC) coupled with time-of-flight mass spectrometry (TOF-MS) and ion trap mass spectrometry (IT-MS) is well-suited to be performed as qualitative analysis tool in this field. The purpose of this review is to provide an overview on the potential of this integrated strategy, including the review of general features of LC-IT-MS and LC-TOF-MS, the advantages of their combination, the common procedures for structure elucidation, the potential of LC-hybrid-IT-TOF/MS and also the summary and discussion of the applications of the integrated strategy for HM qualitative analysis (2006-2011). The advantages and future developments of LC coupled with IT and TOF-MS are highlighted.展开更多
A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography (IC) with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemi...A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography (IC) with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemical oxidationneutralization device (EOND), in which iodide of the sample was oxidized to iodate and the alkaline digestion sample solution was neutralized. Under the optimized conditions, the limits of detection (LOD, S/N = 3) were 2.5 μg/L for fluoride and 20 μg/L for iodate, respectively. The recoveries were in the range of 93-102% for fluoride and 86-98% for iodate.展开更多
Artificial molecular chaperone (AMC) and ion exchange chromatography (IEC) were integrated, thus a new refolding method, artificial molecular chaperone-ion exchange chromatography (AMC-IEC) was developed. Compar...Artificial molecular chaperone (AMC) and ion exchange chromatography (IEC) were integrated, thus a new refolding method, artificial molecular chaperone-ion exchange chromatography (AMC-IEC) was developed. Compared with AMC and IEC, the activity recovery of lysozyme obtained by AMC-IEC was much higher in the investigated range of initial protein concentrations, and the results show that AMC-IEC is very efficient for protein refolding at high concentrations. When the initial concentration of lysozyme is 180 mg/mL, its activity recovery obtained by AMC-IEC is still as high as 76.6%, while the activity recoveries obtained by AMC and IEC are 45.6% and 42.4%, respectively.展开更多
In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate (TDI) in syntheticrubber track by ion chromatography (IC) coupled with an ultraviolet detector setting at 2...In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate (TDI) in syntheticrubber track by ion chromatography (IC) coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine (TDA) which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column (150 mm ×4.0 mm) using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection (LOD, 0.13 μg L^-1) was obtained. Within-day relative standard deviation (R.S.D.) was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.展开更多
Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensi...Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensional liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(2 D-LC/IM-QTOF-MS)enabling four-dimensional separations(2 D-LC,IM,and MS),is proposed.In combination with in-house database-driven automated peak annotation,this strategy was utilized to characterize ginsenosides simultaneously from white ginseng(WG)and red ginseng(RG).An offline 2 DLC system configuring an Xbridge Amide column and an HSS T3 column showed orthogonality 0.76 in the resolution of ginsenosides.Ginsenoside analysis was performed by data-independent high-definition MSE(HDMSE)in the negative ESI mode on a Vion?IMS-QTOF hybrid high-resolution mass spectrometer,which could better resolve ginsenosides than MSEand directly give the CCS information.An in-house ginsenoside database recording 504 known ginsenosides and 58 reference compounds,was established to assist the identification of ginsenosides.Streamlined workflows,by applying UNIFI?to automatedly annotate the HDMSEdata,were proposed.We could separate and characterize 323 ginsenosides(including 286 from WG and 306 from RG),and 125 thereof may have not been isolated from the Panax genus.The established 2 D-LC/IM-QTOF-HDMSEapproach could also act as a magnifier to probe differentiated components between WG and RG.Compared with conventional approaches,this dimensionenhanced strategy could better resolve coeluting herbal components and more efficiently,more reliably identify the multicomponents,which,we believe,offers more possibilities for the systematic exposure and confirmative identification of plant metabolites.展开更多
Multiple acute and chronic toxicity of arsenic species and its mobilisation from geological deposits into ground and drinking water resources is one of the greatest threats to human health. Arsenic speciation analy-si...Multiple acute and chronic toxicity of arsenic species and its mobilisation from geological deposits into ground and drinking water resources is one of the greatest threats to human health. Arsenic speciation analy-sis, mostly done by liquid chromatography, is a challenging task which requires an intense high quality work with respect to extraction, preservation, separation, detection and validation. A growing number of As-spe-cies and low regulatory limits (10 μg/L) may require more than one speciation method preferably performed by species specific procedures and detectors. Beside As-fractionation for special application there are many selective speciation methods based on high performance separation techniques like capillary electrophoreses, gas and liquid chromatography. Both, fractionation and speciation methods are reviewed. However, the focus is on scopes and limits of ion chromatographic separations, the most frequently used methods. Based on IC-principles the methods applied are critically discussed and recommendations given which should result in more robust and reliable As-speciation.展开更多
Retention behavior of U(VI) and Th(IV) as their 2, 6-pyridine dicarboxylic acid (PDCA) complexes on reversed phase and ion exchange (cation, anion and mixed ion exchange) columns was studied and based on the results, ...Retention behavior of U(VI) and Th(IV) as their 2, 6-pyridine dicarboxylic acid (PDCA) complexes on reversed phase and ion exchange (cation, anion and mixed ion exchange) columns was studied and based on the results, a simple ion chromatography method for the determination of trace level thorium in uranium oxide using 0.075mM 2, 6-pyridine dicarboxylic acid (PDCA) and 1M KNO3 in 1.2M HNO3 as eluent (flow rate 1 mL/min)was proposed. The advantage of the developed method is that the separation of uranium matrix is not required prior to the ion chromatographic determination of trace Th. Separation was carried out on a mixed ion exchange stationary phase and a 10?4 M arsenazo (III) solution was used as post column reagent for detecting the separated metal ions. The separation of Th from uranium using PDCA in the present investigation is attributed through cation exchange mechanism. A calibration plot was constructed by following the standard addition method over the concentration range of 0.25 to 10 ppm of Th in the presence of uranium matrix, which resulted in a linear regression coefficient of 0.9978. The precision of the method was better than 5% and the LOD for Th was found to be 0.1ppm (S/N=3). The method has been validated by comparing the results with the results obtained from ICP-MS analysis where the This separated from the uranium matrix. The proposed method is simple, rapid, accurate and cost effective compared to techniques like ICP-MS or ICP-AES and is suitable for the routine kind of analysis.展开更多
A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, ...A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.展开更多
Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimet...Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.展开更多
In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-...In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time. Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.展开更多
Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propa...Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using100 mMpotassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09%-1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08-0.18 mM and 0.26-0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.展开更多
Alkaloids have a variety of bioactivities and great development value in the fields of pharmaceuticals, cosmetics and health food. Column chromatography is a common method for preparing alkaloids. In this paper, the r...Alkaloids have a variety of bioactivities and great development value in the fields of pharmaceuticals, cosmetics and health food. Column chromatography is a common method for preparing alkaloids. In this paper, the research status of the separation and purification of alkaloids from Chinese medicines by column chromatography is reviewed, and the factors that influence the refining of alkaloids via a macroporous adsorption resin, ion exchange resin and silica gel are summarized. The thermodynamic and kinetic modeling methods for the static adsorption of adsorbents are also reviewed in this paper. It is suggested that the modeling method of the column chromatography process be deeply studied to establish a more stringent quality control method for sampling liquid and to strengthen the online detection of the chromatography process to improve the refining effect of alkaloids.展开更多
L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum (ATCC 21799) strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed (SMB) chromatography....L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum (ATCC 21799) strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed (SMB) chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 (g/(g·h)) (per gram resin and per hour) at an eluent flow rate of 10 (mL/min) in fixed-bed chromatography. The results obtained from SMB were 0.11 (g/(g·h)) for L-lysine purification rate and 96% for L-lysine recovery.展开更多
In this research, a glassy carbon electrode modified with the functionalized multi-wall carbon nanotubes(MWNT-COOHs) film was used as an amperometric sensor for the determination of S_2O^(2-)_3, SO^(2-)_3, I^- and SCN...In this research, a glassy carbon electrode modified with the functionalized multi-wall carbon nanotubes(MWNT-COOHs) film was used as an amperometric sensor for the determination of S_2O^(2-)_3, SO^(2-)_3, I^- and SCN^-. The electrochemical behavior of those oxidizable inorganic anions at this modified electrode was studied by means of cyclic voltammetry(CV). The experimental results indicate that the modified electrode exhibits a high electrocatalytic activity towards the oxidation of those anions with a relatively high sensitivity, a good stability and a long-life. Separated by ion chromatography(IC) with 1.25 mmol/L H_2SO_4 as an eluent, those oxidizable anions can be determined by the MWNT-COOHs modified electrode successfully. Under the optimal chromatographic conditions, the detection limits are 1.5×10^(-7) mol/L for S_2O^(2-)_3, 2.5×10^(-7) mol/L for SO^(2-)_3, 1.2×10^(-7) mol/L for I^- and 2.0×10^(-7) mol/L for SCN^-, respectively. The method was applied successfully to the determination of those anions in environmental water展开更多
The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion m...The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.展开更多
文摘Over recent decades, Gampaha district, Sri Lanka, has experienced significant urbanisation and industrial growth, increasing groundwater demand due to limited and polluted surface water resources. In 2013, a community uprising in Rathupaswala, a village in Gampaha district, accused a latex glove manufacturing factory of causing groundwater acidity (pH < 4). This study evaluates the spatial and temporal changes in geochemical parameters across three transects in the southern part of Gampaha district to 1) assess the impact of geological formations on groundwater;2) compare temporal variations in groundwater;and 3) explain acidification via a geochemical model. Seventy-two sample locations were tested for pH, electrical conductivity (EC), and anion concentrations (sulphate, nitrate, chloride and fluoride). Depth to the water table and distance from the sea were measured to study variations across sandy, peaty, lateritic, and crystalline aquifers. Results showed pH readings around 7 for sandy and crystalline aquifers, below 7 for peaty aquifers, and below 5 for lateritic aquifers, with significant water table fluctuations near Rathupaswala area. Principal component analysis revealed three principal components (PCs) explaining 86.0% of the variance. PC1 (40.6%) correlated with pH, EC, and sulphate (saltwater intrusion), while PC2 (32.0%) correlated with nitrates and depth to the water table (anthropogenic nutrient pollution). A geochemical transport model indicated a cone of depression recharged by acidic groundwater from peat-soil aquifers, leading to acidic groundwater in Rathupaswala area. Previous attributions of acidic pH to the over-exploitation of groundwater by the latex factory have been reevaluated;the results suggest natural acidification from prolonged water-rock interactions with iron-rich lateritic aquifers. Groundwater pH is influenced by local climate, geology, topography, and drainage systems. It is recommended that similar water-rock interaction conditions may be present throughout the wet zone of Sri Lanka, warranting detailed studies to confirm this hypothesis.
基金Supported by Changsha Key Project in Hunan Province(K1005007-21)~~
文摘[Objective] The aim was to analyze sugar components in fermented rice wine by ion chromatography. [Method] The optimal condition for chromatography system of sugar analysis was selected by measuring sugars in fermented rice wine with ion chromatography and pulsed amperometric detection. [Result] The optimal measurement conditions were as follows: Leacheate (Leachate), consisting of NaOH and CH3COONa, was eluted by gradient concentrations, with column temperature at 35 ℃ and flow rate at 0.4 ml/min. In the condition, sugars in rice wine were ana- lyzed and the results showed that the method is featured by low detection limit, good repetition and high recovery rate. [Conclusion] The research establishes and determines the approaches and optimum conditions for sugar analysis in rice wine by ion chromatography and pulsed amperometric detection, providing references for advancement of research on quality improvement of fermented rice wine.
基金Project supported by the Hi-Tech Research and Development Program(863) of China (No. 2003AA601130).
文摘The ion chromatography combined solid phase extraction (SPE) method was developed for the analysis of low concentration haloacetic acids (HAAs), a class of disinfection by-products formed from chlorination of hospital wastewater. The monitored HAAs included monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, dibromoacetic acid and trichloroacetic acid. The method employed a sodium hydroxide eluent at a flow rate of 0.8 ml/min, electrolytically generated gradients, and suppressed conductivity detection. To analyze the HAAs in real hospital wastewater samples, C18 pretreatment cartridge was utilized to reduce samples' turbidity. Preconcentration with SPE and matrix elimination with treatment cartridges were investigated and found to be able to obtain acceptable detection limits. Linearity, repeatability and detection limits of the above method were evaluated. The detection limits of monobromoacetic acid and dibromoacetic acid were 2.61 μg/L and 1.30 μg/L, respectively, and the other three acids are ranging from 0.48 to 0.82μg/L under 25-fold preconcentration. When the above optimization procedure was applied to three hospital wastewater samples with different treatment processes in Tianjin, it was found that the dichloroacetic acid was the major compound, and the growth ratios of the HAAs after disinfection by sodium hypochlorite were 91.28%, 63.61% and 79.50%, respectively.
文摘A simple, sensitive and convenient ion chromatography(IC) method was established for the simultaneous determination of twelve water-soluble inorganic anions(F -, Cl -, NO - 2, NO - 3, SO 2- 3, SO 2- 4, PO 3- 4), and fifteen water-soluble organic ions(formate, acetate, MSA, oxalate, malonate, succinate, phthalates, etc.) in atmospheric aerosols. The linear concentrations ranged from 0.005 μg/m 3 to 500 μg/m 3(r = 0.999—0.9999). The relative standard deviation(RSD) were 0.43%—2.00% and the detection limits were from 2.7 ng/m 3 to 88 ng/m 3. The proposed method was successfully applied to the simultaneous determination of those inorganic ions and organic ions in PM 2.5 of Beijing.
文摘With the expansion of herbal medicine (HM) market, the issue on how to apply up-to- date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention. Due to its inherent characteristics of accurate mass measurements and multiple stages analysis, the integrated strategy of liquid chromatography (LC) coupled with time-of-flight mass spectrometry (TOF-MS) and ion trap mass spectrometry (IT-MS) is well-suited to be performed as qualitative analysis tool in this field. The purpose of this review is to provide an overview on the potential of this integrated strategy, including the review of general features of LC-IT-MS and LC-TOF-MS, the advantages of their combination, the common procedures for structure elucidation, the potential of LC-hybrid-IT-TOF/MS and also the summary and discussion of the applications of the integrated strategy for HM qualitative analysis (2006-2011). The advantages and future developments of LC coupled with IT and TOF-MS are highlighted.
文摘A new method for the simultaneous determination of fluorine and iodine in urine by ion chromatography (IC) with electrochemical pretreatment has been developed. The pretreatment was performed in a novel electrochemical oxidationneutralization device (EOND), in which iodide of the sample was oxidized to iodate and the alkaline digestion sample solution was neutralized. Under the optimized conditions, the limits of detection (LOD, S/N = 3) were 2.5 μg/L for fluoride and 20 μg/L for iodate, respectively. The recoveries were in the range of 93-102% for fluoride and 86-98% for iodate.
基金the National Natural Science Foundation in China(No.20705028)the Foundation of Key Laboratory of Modem Separation Science in Shaanxi Province(No.05JS61).
文摘Artificial molecular chaperone (AMC) and ion exchange chromatography (IEC) were integrated, thus a new refolding method, artificial molecular chaperone-ion exchange chromatography (AMC-IEC) was developed. Compared with AMC and IEC, the activity recovery of lysozyme obtained by AMC-IEC was much higher in the investigated range of initial protein concentrations, and the results show that AMC-IEC is very efficient for protein refolding at high concentrations. When the initial concentration of lysozyme is 180 mg/mL, its activity recovery obtained by AMC-IEC is still as high as 76.6%, while the activity recoveries obtained by AMC and IEC are 45.6% and 42.4%, respectively.
基金supported by the National Natural Science Foundation of China(No.20775070)Zhejiang Provincial Natural Science Foundation of China(No.Y507252).
文摘In the present work, a novel analytical method was proposed for the determination of toluene diisocyanate (TDI) in syntheticrubber track by ion chromatography (IC) coupled with an ultraviolet detector setting at 212 nm. TDI can be hydrolyzed to toluene diamine (TDA) which can be separated by cation-exchange IC easily. The optimum IC separation was performed on an IonPac CS12A column (150 mm ×4.0 mm) using 20 mmol L^-1 sodium sulfate, 10 mmol L^-1 sulfuric acid and 10% acetonitrile as eluent. It was found that a higher signal response of TDA could be obtained under alkaline condition. A suppressor was used to change the acidic eluent into alkaline one. 0.8 mol L^-1 potassium hydroxide was chosen as the optimum regeneration eluent. With the added suppressor and regenerant, signal response was magnified by about 16 times and lower limit of detection (LOD, 0.13 μg L^-1) was obtained. Within-day relative standard deviation (R.S.D.) was less than 3.6%. The recoveries of TDI spiked in synthetic-rubber track samoles were 96.4-110.6%.
基金the National Natural Science Foundation of China(Grant No.81872996)the State Key Research and Development Project(Grant No.2017YFC1702104)+1 种基金the State Key Project for the Creation of Major New Drugs(2018ZX09711001-009-010)the Tianjin Municipal Education Commission Research Project(Grant No.2017ZD07)。
文摘Inherent complexity of plant metabolites necessitates the use of multi-dimensional information to accomplish comprehensive profiling and confirmative identification.A dimension-enhanced strategy,by offline two-dimensional liquid chromatography/ion mobility-quadrupole time-of-flight mass spectrometry(2 D-LC/IM-QTOF-MS)enabling four-dimensional separations(2 D-LC,IM,and MS),is proposed.In combination with in-house database-driven automated peak annotation,this strategy was utilized to characterize ginsenosides simultaneously from white ginseng(WG)and red ginseng(RG).An offline 2 DLC system configuring an Xbridge Amide column and an HSS T3 column showed orthogonality 0.76 in the resolution of ginsenosides.Ginsenoside analysis was performed by data-independent high-definition MSE(HDMSE)in the negative ESI mode on a Vion?IMS-QTOF hybrid high-resolution mass spectrometer,which could better resolve ginsenosides than MSEand directly give the CCS information.An in-house ginsenoside database recording 504 known ginsenosides and 58 reference compounds,was established to assist the identification of ginsenosides.Streamlined workflows,by applying UNIFI?to automatedly annotate the HDMSEdata,were proposed.We could separate and characterize 323 ginsenosides(including 286 from WG and 306 from RG),and 125 thereof may have not been isolated from the Panax genus.The established 2 D-LC/IM-QTOF-HDMSEapproach could also act as a magnifier to probe differentiated components between WG and RG.Compared with conventional approaches,this dimensionenhanced strategy could better resolve coeluting herbal components and more efficiently,more reliably identify the multicomponents,which,we believe,offers more possibilities for the systematic exposure and confirmative identification of plant metabolites.
文摘Multiple acute and chronic toxicity of arsenic species and its mobilisation from geological deposits into ground and drinking water resources is one of the greatest threats to human health. Arsenic speciation analy-sis, mostly done by liquid chromatography, is a challenging task which requires an intense high quality work with respect to extraction, preservation, separation, detection and validation. A growing number of As-spe-cies and low regulatory limits (10 μg/L) may require more than one speciation method preferably performed by species specific procedures and detectors. Beside As-fractionation for special application there are many selective speciation methods based on high performance separation techniques like capillary electrophoreses, gas and liquid chromatography. Both, fractionation and speciation methods are reviewed. However, the focus is on scopes and limits of ion chromatographic separations, the most frequently used methods. Based on IC-principles the methods applied are critically discussed and recommendations given which should result in more robust and reliable As-speciation.
文摘Retention behavior of U(VI) and Th(IV) as their 2, 6-pyridine dicarboxylic acid (PDCA) complexes on reversed phase and ion exchange (cation, anion and mixed ion exchange) columns was studied and based on the results, a simple ion chromatography method for the determination of trace level thorium in uranium oxide using 0.075mM 2, 6-pyridine dicarboxylic acid (PDCA) and 1M KNO3 in 1.2M HNO3 as eluent (flow rate 1 mL/min)was proposed. The advantage of the developed method is that the separation of uranium matrix is not required prior to the ion chromatographic determination of trace Th. Separation was carried out on a mixed ion exchange stationary phase and a 10?4 M arsenazo (III) solution was used as post column reagent for detecting the separated metal ions. The separation of Th from uranium using PDCA in the present investigation is attributed through cation exchange mechanism. A calibration plot was constructed by following the standard addition method over the concentration range of 0.25 to 10 ppm of Th in the presence of uranium matrix, which resulted in a linear regression coefficient of 0.9978. The precision of the method was better than 5% and the LOD for Th was found to be 0.1ppm (S/N=3). The method has been validated by comparing the results with the results obtained from ICP-MS analysis where the This separated from the uranium matrix. The proposed method is simple, rapid, accurate and cost effective compared to techniques like ICP-MS or ICP-AES and is suitable for the routine kind of analysis.
基金Project(2005CB623702) supported by the National Key Basic Research Program of China
文摘A method for the simultaneous separation and determination of organic acids and inorganic anions in Bayer liquors was developed by gradient ion chromatography with suppressed conductivity detection. Formate, acetate, propionate, oxalate, succinate, glutarate, fluoride, chloride and sulfate were separated and determined in 33 min. The samples were pretreated with solid-phase extraction, which has high selectivity for removing a large number of metallic ions in the Bayer liquors, and filtered with a 0.45 μm filter membrane before being injected into the ion chromatographic system. The separation of six organic acids and three inorganic anions was achieved on an IonPac AS11-HC column with KOH as the eluent, and the detection was performed by a conductivity detection mode. No interference is found in the presence of fluorate, chlorate and sulphate when organic acids are determined. The calibration graphs of peak area for all the analytes are linear over a wide range. The relative standard derivation of the peak area of analytes is less than 2.14%. Under optimum conditions the detection ranges from 0.2 to 100.0 mg/L. The average recoveries of the added standards are between 94.3% and 102.8%.
基金funded by the National Major ScientificInstrument and Equipment Development Project of China (No.2012YQ090229)
文摘Ion chromatography-ultra violet-hydride generation-Atomic Florescence Spectrometry was applied to detect 5 arsenic species in seafoods. The arsenic species studied include arsenobetaine(As B), arsenite(As(III)), dimethylarsinic acid(DMA), monomethylarsonic acid(MMA), and arsenate(As(V)), which were extracted from samples using 2% formic acid. Gradient elution using 33 mmol L^(-1) CH_3COONH_4 and 15 mmol L^(-1) Na_2CO_3 with 10 mL CH_3CH_2OH at pH 8.4 allowed the chromatographic separation of all the species on a Hamilton PRP-X100 anion-exchange column in less than 8 min. In this study, an ultrasound extraction method was used to extract arsenic species from seafood. The extraction efficiency was good and the recoveries from spiked samples were in the range of 72.6%–109%; the precision between sample replicates was higher than 3.6% for all determinations. The detection limits were 3.543 μg L^(-1) for As B, 0.4261 μg L^(-1) for As(III), 0.216 μg L^(-1) for DMA, 0.211 μg L^(-1) for MMA, and 0.709 μg L^(-1) for As(V), and the linear coefficients were greater than 0.999. We also developed an application of this method for the determination of arsenic species in bonito, Euphausia superba, and Enteromorpha with satisfactory results. Therefore, it was confirmed that this method was appropriate for the detection of arsenic species in seafood.
基金supported by National Natural Science Foundation of China(No.20775070)by Zhejiang Provincial Natural Science Foundation of China(No.R4080124)Zhejiang Qianjiang Project of Science and Technology for Competent People(No.2008R10028).
文摘In this work, a novel hollow fiber membrane extractor was set up to extract inorganic anions from ethyl acetate using deionized water. Inorganic anions in slightly soluble organic solvents can be determined by the in-line hollow fiber membrane extractor coupled with ion chromatography at first time. Different aspects of the extraction procedure such as magnetic stirring speed, extraction flow rate and extraction time were optimized to achieve high extraction efficiency and good separation results. Satisfactory linear range, limits of detection and good repeatability were obtained. The procedure was applied to analyze inorganic anions in two commercial ethyl acetate samples.
文摘Methacrylate-based monolithic column was prepared in fused-silica capillary (80 ′ 0.32 mm i.d.) by in situ polymerizetion reaction using glycidyl methacrylate as monomer;ethylene dimethacrylate as crosslinker;1-propanol, 1,4-butanediol, and water as porogenic solvents. The monolith matrix was modified with trimethylamine to create strong anion exchanger via ring opening reaction of epoxy groups. The morphology of the monolithic column was studied by using Scanning Electron Microscope (SEM). This column had good mechanical stability and permeability. The effects of various mobile phases for separation of inorganic anions were investigated. Iodate, bromate, nitrite, bromide, and nitrate were separated within 11 min using100 mMpotassium chloride as mobile phase and detected at 210 nm. This method showed good precision of retention time, acceptable linearity and good sensitivity. Under the optimum condition, the RSD of the retention time was in the range of 1.09%-1.75% (n = 6). The calibration curve showed linear relationships between the peak area and the concentration. The limits of detection (LOD) and the limits of quantitation (LOQ) were between 0.08-0.18 mM and 0.26-0.61 mM, respectively. This method was applied to the determination of inorganic anions in tap water and ground water samples.
文摘Alkaloids have a variety of bioactivities and great development value in the fields of pharmaceuticals, cosmetics and health food. Column chromatography is a common method for preparing alkaloids. In this paper, the research status of the separation and purification of alkaloids from Chinese medicines by column chromatography is reviewed, and the factors that influence the refining of alkaloids via a macroporous adsorption resin, ion exchange resin and silica gel are summarized. The thermodynamic and kinetic modeling methods for the static adsorption of adsorbents are also reviewed in this paper. It is suggested that the modeling method of the column chromatography process be deeply studied to establish a more stringent quality control method for sampling liquid and to strengthen the online detection of the chromatography process to improve the refining effect of alkaloids.
文摘L-Lysine was produced by a microbial process utilizing a Corynebacterium glutamicum (ATCC 21799) strain. L-Lysine was purified from the cultivated medium by fixed-bed and simulated moving bed (SMB) chromatography. The separation conditions including pH, eluent concentration and Lys+ and Lys2+ adsorption isotherms were studied in batch adsorption. The column capacity, eluent flow rate and eluent concentration have been studied in fixed-bed chromatography. Maximum purification rate of lysine was obtained as 0.066 (g/(g·h)) (per gram resin and per hour) at an eluent flow rate of 10 (mL/min) in fixed-bed chromatography. The results obtained from SMB were 0.11 (g/(g·h)) for L-lysine purification rate and 96% for L-lysine recovery.
基金supported by the National Natural Science Foundation of China(No.2 0 175 0 0 6 ) and Nano Projects from Shanghai Sci-ence and Technology Com mittee(No.0 2 14 nm0 78and0 35 9nm0 0 2 )
文摘In this research, a glassy carbon electrode modified with the functionalized multi-wall carbon nanotubes(MWNT-COOHs) film was used as an amperometric sensor for the determination of S_2O^(2-)_3, SO^(2-)_3, I^- and SCN^-. The electrochemical behavior of those oxidizable inorganic anions at this modified electrode was studied by means of cyclic voltammetry(CV). The experimental results indicate that the modified electrode exhibits a high electrocatalytic activity towards the oxidation of those anions with a relatively high sensitivity, a good stability and a long-life. Separated by ion chromatography(IC) with 1.25 mmol/L H_2SO_4 as an eluent, those oxidizable anions can be determined by the MWNT-COOHs modified electrode successfully. Under the optimal chromatographic conditions, the detection limits are 1.5×10^(-7) mol/L for S_2O^(2-)_3, 2.5×10^(-7) mol/L for SO^(2-)_3, 1.2×10^(-7) mol/L for I^- and 2.0×10^(-7) mol/L for SCN^-, respectively. The method was applied successfully to the determination of those anions in environmental water
文摘The application of non-suppressed ion chromatography for monitoring of trace elements in air particulate matter was studied in the present investigation. The results indicate that the use of microwave acid digestion method is superior in comparison with the conventional thermal acid digestion method as it leads to higher recovery, better reproducibility, lower volatility loss, better protection against environmental contamination and much less digestion time (5 minutes vs. 24 hours). The use of eluent as extractant is shown to reduce the water dip problem in the chro-matogram. The addition of chelating agent in the eluent coupled with UV detection is shown to provide satisfactory chromatographic separation and good sensitivity for the analysis of transition metals present in the air particulate matter. Using the U.S. National Bureau of Standards Reference Material 1648 Urban Particulate Matter as standard for checking, the analytical procedure is shown to give good recovery and reproducibility for the detection of the following cations and anions in air particulate matter: Fe2 Cu, Mn, Pb, Zn, Mg, Na, HN4+, Cl-, NO3- and SO42-. Field test was also performed to check the applicability of the method and the results obtained were discussed in the present paper.