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1.
In this work, an analytical methodological study was carried out to determine the antimicrobials sulfamethoxazole and trimethoprim, as well as their metabolites, in hospital effluent. The determinations were conducted by liquid chromatography tandem mass spectrometry using a hybrid triple quadrupole‐linear ion trap mass spectrometer (LC‐QqLIT‐MS). The data acquisition was made in selected reaction monitoring (SRM) mode, in which two SRM transitions were monitored to ensure that the target compounds were accurately identified by the information dependent acquisition (IDA) function. The limits of detection (LOD) and quantification (LOQ) were 0.25 and 0.80 µg L?1 for sulfamethoxazole and 0.15 and 0.50 µg L?1 for trimethoprim. The linear range for the SMX was 0.8–100.0 µg L?1 and TMP was 0.5–100.0 µg L?1 on the basis of six‐point calibration curves generated by means of linear regression analysis. The coefficients of the correlation were higher than 0.999, which ensured the linearity of the method. The average concentration of sulfamethoxazole and trimethoprim found in hospital effluent was 27.8 and 6.65 µg L?1, respectively. The analytical methodology employed allowed two metabolites to be identified, N4‐acetyl‐sulfamethoxazole and α‐hydroxy‐trimethoprim. Fragmentation pathways were proposed.  相似文献   

2.
In this study the occurrence of diclofenac and sub‐products in effluent emerging from the University Hospital at the Federal University of Santa Maria was investigated. One metabolite was identified and, in aqueous solution, three degradation products. The quantification was conducted by means of HPLC‐DAD, and the determination of metabolite and degradation products by LC–ESI–MS/MS–QTrap. For the HPLC‐DAD method, a 70:30 mixture of methanol/sodium phosphate was used in isocratic mode. For the LC–ESI–MS/MS–QTrap determinations, a mobile phase, where phase A was an ammonium acetate solution 5 × 10?3 mol L?1, and phase B was methanol (5 × 10?3 mol L?1)/ammonium acetate (9:1, v/v), on gradient mode. The LDs for the HPLC and LC–MS/MS methods, respectively, were 2.5 and 0.02 µg L?1, the LQs, 8.3 and 0.05 µg L?1, and the linear range from 10 up to 2000 µg L?1 and 0.05 up to 10 µg L?1. As expected, the LC–ESI–MS/MS–QTrap method was more sensitive and less laborious. The metabolite 4′‐hydroxy‐diclofenac was identified. Photolysis was used for the degradation studies and three products of diclofenac were identified (m/z of 214, 286 and 303) in aqueous solution. These results notwithstanding, no degradation products of diclofenac were found in the hospital effluent.  相似文献   

3.
The aim of this study is to investigate the concentrations of U, Th, V, Mo, and Zr in natural waters taken from Turkey. Among these water species, Lake Van is the largest soda lake and the fourth largest closed basin on Earth. The water samples were collected from 51 locations between 2008 and 2009. The inductively coupled plasma‐MS was used for determinations. The obtained U and Zr concentrations are in the range of 37–110 µg L?1 and 17–78 µg L?1 in Lake Van and 0.53–0.81 µg L?1 and 0.15–0.19 µg L?1 in Lake Hazar, respectively. The concentration of uranium in other studied waters varies from the lowest 0.09 µg L?1 in Tigris (Dicle) river to the highest 4.0 µg L?1 in Mediterranean Sea water. Mean Mo and V concentrations in the studied water samples were found to be in ranges of 0.1–17 and 2.7–113 µg L?1, respectively. The obtained highest U concentration in Lake Van correlates with the highest Mo and Zr levels compared to the Lake Hazar and river waters. These results imply that there is a young occurrence of uranium minerals around Lake Van. It is concluded that there is about 50.000 ton of uranium in Lake Van water.  相似文献   

4.
A simple and reliable method for rapid and selective extraction and determination of trace levels of Ni2+ and Mn2+ was developed by ionic liquid (IL) based dispersive liquid–liquid microextraction coupled to flame atomic absorption spectrometry (FAAS) detection. The proposed method was successfully applied to the preconcentration and determination of nickel and manganese in soil, vegetable, and water samples. After preconcentration, the settled IL‐phase was dissolved in 100 µL of ethanol and aspirated into the FAAS using a home‐made microsample introduction system. Injection of 50 µL of each analyte into an air–acetylene flame provided very sensitive spike‐like and reproducible signals. Effective parameters such as pH, amount of IL, volume of the disperser solvent, concentration of the chelating agent, and effect of salt concentration were inspected by a (25‐1) fractional factorial design to identify the most important parameters and their interactions. Under optimum conditions, preconcentration of 10 mL sample solution permitted the detection of 0.93 µg L?1 Ni2+ and 0.52 µg L?1 Mn2+ with enrichment factors 77.2 and 82.6 for Ni2+ and Mn2+, respectively. The accuracy of the procedure was evaluated by analysis of a certified reference material (CRM TMDW‐500, drinking water).  相似文献   

5.
Simple, rapid, and sensitive spectrophotometric methods have been proposed for the determination of cationic surfactants (CS) as cetyltrimethylammonium bromide (CTAB), dodecyltrimethylammonium (DTAB), and cetylpyridinium bromide (CPB). The methods are based on the effects of CSs on the complexes of Al3+ and Be2+ with Chrome Azurol S (CAS). The optimum reaction conditions such as CAS concentration, metal ion concentration, and pH have been studied and found to be 2.0 × 10?4 mol L?1 CAS, 0.5 mg L?1 Al3+ or 0.4 mg L?1 Be2+ and pH 5.4. The analytical characteristics of the methods such as limit of detections, limit of quantifications, and linear ranges have been obtained. CTAB, CPB, and DTAB could be determined by the Al–CAS complex in the ranges of 0.50–40.00, 0.20–10.00, and 0.40–10.00 µmol L?1, and for the Be–CAS complex in the ranges of 0.08–5.00, 0.08–3.00, and 0.20–6.00 µmol L?1, respectively. The limit of the detections of the method for the determination of CTAB, CPB, and DTAB for the Be–CAS complex has been found as 0.025, 0.024, and 0.061 µmol L?1, respectively. The interfering effect of some anions and cations was also tested. The method was applied to the determination of CS CTAB in conditioner shampoo and water samples.  相似文献   

6.
Bezafibrate (BZF), a widely used lipid regulator, is a potential threat to ecosystems and human health in water, and the recent research showed that advanced oxidation processes (AOPs) are much more effective for BZF degradation. In this study, we investigated the photochemical decomposition of BZF in surface water and effluent from waste water treatment plants (WWTP) by UV/H2O2 process. The results showed that the UV/H2O2 process was a promising method to remove BZF at low concentration, generally at µg L?1 level. When initial concentrations reach 100 µg L?1 in the deionized water, >99.8% of BZF could be removed in 16 min under UV intensity of 61.4 µm cm?2, at the H2O2 concentration of 0.1 mg L?1, and neutral pH condition. Moreover, BZF degradation was inhibited in this process when humic acid (HA) and inorganic solution anions were added to the deionized water solutions, including chloride, nitrate, bicarbonate, and sulfate, significantly. In the surface water and effluent of WWTP, however, the removal efficiency of BZF was lower than that in the deionized water because of the interference of complex constituents in the surface water and effluent. Some main intermediates at the m/z range of 100–400 were observed by high performance LC‐MS (HPLC/MS) and a simple pathway of BZF degradation by UV/H2O2 was proposed.  相似文献   

7.
The coprecipitation method is widely used for the preconcentration of trace metal ions prior to their determination by flame atomic absorption spectrometry (FAAS). A simple and sensitive method based on coprecipitation of Fe(III) and Ni(II) ions with Cu(II)‐4‐(2‐pyridylazo)‐resorcinol was developed. The analytical parameters including pH, amount of copper (II), amount of reagent, sample volume, etc., were examined. It was found that the metal ions studied were quantitatively coprecipitated in the pH range of 5.0–6.5. The detection limits (DL) (n = 10, 3s/b) were found to be 0.68 µg L?1 for Fe(III) and 0.43 µg L?1 for Ni(II) and the relative standard deviations (RSD) were ≤4.0%. The proposed method was validated by the analysis of three certified reference materials (TMDA 54.4 fortified lake water, SRM 1568a rice flour, and GBW07605 tea) and recovery tests. The method was successfully applied to sea water, lake water, and various food samples.  相似文献   

8.
Cyanuric acid is a suspected gastrointestinal or liver toxicant in humans. Therefore, determination of trace cyanuric acid is very important, in this work a novel, sensitive, and reliable method was developed using differential pulse polarography. Optimum conditions for analytical determination were found to be at a pH of 9.5, Britton–Robinson at a reduction potential of ?105 mV. Experimental results indicate an excellent linear correlation between the peak current and the concentration in the range of cyanuric acid from 0.5 to 27.0 µM (0.06–3.5 µg mL?1) with a correlation coefficient of 0.997. The limit of detection and limit of quantification were obtained as 0.15 and 0.5 µM (0.02–0.06 µg mL?1), respectively. The proposed method was successfully applied to the determination of cyanuric acid in pool water and in spiked milk. Cyanuric acid level in swimming pool water was found as 2.54 ± 0.47 µg mL?1 (19.7 ± 2.29 µM) in swimming pool water for N = 4 and 95% confidence interval. The recoveries were found to be sufficient. Also, the standard deviation of the data was low which shows high accuracy and precision of proposed differential pulse polarographic method. The influences of some other commonly found inorganic salts on the determination of cyanuric acid were also examined. Some interfering species were eliminated using complexing agents, e.g., EDTA.  相似文献   

9.
Cadmium (Cd) has become an important heavy metal contaminant in the sediment and seawater along the Bohai Sea and been of great ecological risk due to its toxic effects to marine organisms. In this work, the toxicological effects caused by environmentally relevant concentrations (10 and 40 µg L?1) of Cd were studied in the gill tissues of Manila clam Ruditapes philippinarum after exposure for 24, 48, and 96 h. Both low (10 µg L?1) and high (40 µg L?1) doses of Cd caused the disturbances in energy metabolism and osmotic regulation and neurotoxicity based on the metabolic biomarkers such as succinate, alanine, branched chain amino acids, betaine, hypotaurine, and glutamate in clam gills after 24 h of exposure. However, the recovery of toxicological effects of Cd after exposure for 96 h was obviously observed in clam to Cd exposures. Overall, these results indicated that NMR‐based metabolomics was applicable to elucidate the toxicological effects of heavy metal contaminants in the marine bioindicator.  相似文献   

10.
An on‐line solid phase extraction method for the preconcentration and determination of Cu(II) by flame atomic absorption spectrometry has been described. The procedure is based on the retention of Cu(II) ions at pH 6.0 on a minicolumn packed with Amberlite XAD‐1180 resin impregnated with chrome azurol S. After preconcentration, Cu(II) ions adsorbed on the impregnated resin were eluted by 1 mol L?1 HNO3 solution. Several parameters, such as pH, type of eluent, flow rates of sample and eluent solutions, amount of resin were evaluated. At optimized conditions, for 3.5 min of preconcentration time, the system achieved a detection limit of 1.0 µg L?1, and a relative standard deviation of 1.2% at 0.2 µg mL?1 copper. An enrichment factor of 56‐fold was obtained with respect to the copper determination. The proposed method was successfully validated by the analysis of standard reference material (TMDA 54.4 lake water) and recovery studies. The method was applied to the preconcentration of Cu(II) in natural water samples.  相似文献   

11.
Dispersive liquid–liquid microextraction based on solidification of floating organic droplet (DLLME‐SFO) technique was successfully applied for simultaneous assay of eight polychlorinated biphenyls, two organochlorine, and four pyrethroid pesticides multi‐residue in aqueous samples by using GC‐electron capture detection. The effects of various parameters such as kind of extractant and dispersant and volume of them, extraction time, effect of salt addition, and pH were optimized. As a result, 5.0 µL 1‐dodecanol was chosen as extraction solvent, 600 µL methanol were used as dispersive solvent without salt addition, pH was adjusted to 7. Under the optimized conditions, the limits of detection (LOD) were ranged from 1.4 to 8.3 ng L?1. Satisfactory linear range was observed from 5.0 to 2000 ng L?1 with correlation coefficient better than 0.9909. Good precisions were also acquired with RSD better than 13.6% for all target analytes. The enrichment factors of the method were ranged from 786 to 1427. The method can be successfully applied to simultaneous separation and determination of three class residues in real water samples and good recoveries were obtained ranging from 76 to 130, 73 to 129, and 78 to 130% for tap water, lake water, and industrial waste water, respectively.  相似文献   

12.
Malachite green (MG), a traditional agent used in aquaculture although is not approved; its low cost and high efficacy make illicit use likely. We developed a small‐scale, simple, and sensitive dispersive liquid–liquid microextraction procedure for the assay of trace amounts of MG in aquatic environment of Trout fish. Fiber optic‐linear array detection spectrophotometry with charge‐coupled device detector benefiting from a microcell was used for this purpose. The method is based on enhancement effect of an anionic surfactant on the extraction of MG in to very fine multidroplets of microextraction solvent which made assisted by disperser solvent. Under the optimum conditions, the enrichment factor 77.5 was obtained from a 5‐mL water sample. The calibration graph was linear up to 5 × 10?7 mol L?1 with detection limit of 1 × 10?8 mol L?1. The relative standard deviation for seven replicate measurements of 4 × 10?7 and 5 × 10?8 mol L?1 of MG were 3.3 and 4.5%, respectively.  相似文献   

13.
This study examines the effect of drawdown on the timing and magnitude of suspended solids and associated phosphorus export from a 12 ha reservoir located in an urbanized watershed in southern Ontario, Canada. Water level in Columbia Lake was lowered by 1·15 m over a 2‐week period in November 2001. The total phosphorus (TP) concentrations ranged from 63 to 486 µg L?1 in Columbia Lake and 71 to 373 µg L?1 at its outflow. All samples exceeded the Provincial Water Quality Objective of 30 µg TP L?1. Outflow concentrations of suspended solids and TP increased significantly with decreasing lake level and were attributed to the resuspension of cohesive bottom sediments that occurred at a critical threshold lake level (0·65 m below summer level). Suspended solids at the outflow consisted of flocculated cohesive materials with a median diameter (D50) of c. 5 µm. Particulate organic carbon accounted for 8·5% of the suspended solids export by mass. A total mass of 18·5 t of suspended solids and 62·6 kg TP was exported from Columbia Lake, which represents a significant pulse of sediment‐associated P to downstream environments each autumn during drawdown. The downstream impacts of this release can be minimized if the water level in Columbia Lake is lowered no more than 0·5 m below summer levels. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

14.
A method for the determination of nickel in water was developed. The procedure involves preconcentration of nickel by using dispersive liquid–liquid microextraction. The Ni(II) ions were extracted in chloroform in the form of complex with the reagent 2‐(2′‐benzothiazolylazo)‐p‐cresol. Ethanol was used as the disperser solvent. After injection of the extracting mixture in a solution of nickel, a cloudy mixture was observed. A quick centrifugation induces phase separation and thus the settling of rich phase. The nickel content in the rich phase is measured by flame atomic absorption spectrometry. Under optimal conditions, the limit of detection and quantification obtained were 1.4 and 4.7 µg L?1, respectively. Some parameters used to characterize preconcentration systems, such as enrichment factor and consumption index were calculated and resulted in 29 and 0.34 mL, respectively. After optimization of variables and determination of analytical characteristics, the method was used for the analysis of certified reference materials (BCR‐713: wastewater, effluent and BCR‐414: plankton) and real water samples.  相似文献   

15.
The rigin and fate of six phthalate esters (dimethyl phthalate (DMP), diethyl phthalate (DEP), di‐n‐butyl phthalate (DnBP), butyl benzyl phthalate (BBP), di (2‐ethylhexyl) phthalate (DEHP) and di‐n‐octyl phthalate (DnOP)), were investigated during 2005 and 2006 in the densely populated Seine river estuary. Four compounds, DMP, DEP, DnBP and DEHP were detected at all the stations with DEHP (160–314 ng L?1), followed by DEP (71–181 ng L?1) and next DnBP (67–319 ng L?1), except at la Bouille, where DnBP was the second most important compound. BBP and DnOP concentrations remained low and were not found at all the stations. Considering all six phthalates, Caudebec‐en‐Caux (beginning of the salinity gradient) was the least polluted station (464 ng L?1), whereas Honfleur (771 ng L?1) and La Bouille (716 ng L?1) displayed the highest contamination levels, probably related to important industrial plants. From Caudebec‐en‐Caux to Honfleur (maximum turbidity), variation of DEHP concentration was related to that of suspended matter. In addition, the salinity rise in that area might have facilitated DEHP sorption upon particles. A significant correlation between flow magnitude and DEHP concentration was found (P < 0·01, n = 12), supporting the influence of the hydrological cycle upon contamination. Runoff contribution (56·9 kg d?1) to river contamination was confirmed by the annual evolution of phthalate concentrations in the Seine river at Poses. Concentrations of DEHP in the tributaries were in the same range as those of the Seine River (100–350 ng L?1), except for two in densely populated and industrialized areas: Robec (800 ng L?1) and Cailly (970 ng L?1). The treatment plant discharge fluxes were in the same range as those of tributaries (30·4–250 g d?1). During high flow periods, the influence of tributaries and of treatment plants seemed to play a minor part in the contamination level of the Seine river estuary. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

16.
Here we characterize the nutrient content in the outflow of the Green Lake 5 rock glacier, located in the Green Lakes Valley of the Colorado Front Range. Dissolved organic carbon (DOC) was present in all samples with a mean concentration of 0·85 mg L?1 . A one‐way analysis of variance test shows no statistical difference in DOC amounts among surface waters (p = 0·42). Average nitrate concentrations were 69 µmoles L?1 in the outflow of the rock glacier, compared to 7 µmoles L?1 in snow and 25 µmoles L?1 in rain. Nitrate concentrations from the rock glacier generally increased with time, with maximum concentrations of 135 µmoles L?1 in October, among the highest nitrate concentrations reported for high‐elevation surface waters. These high nitrate concentrations appear to be characteristic of rock glacier outflow in the Rocky Mountains, as a paired‐difference t‐test shows that nitrate concentrations from the outflow of 7 additional rock glaciers were significantly greater compared to their reference streams (p = 0·003). End‐member mixing analysis suggest that snow was the dominant source of nitrate in June, ‘soil’ solution was the dominant nitrate source in July, and base flow was the dominant source in September. Fluoresence index values and PARAFAC analyses of dissolved organic matter (DOM) are also consistent with a switch from terrestrial DOM in the summer time period to an increasing aquatic‐like microbial source during the autumn months. Copyright © 2006 John Wiley & Sons, Ltd.  相似文献   

17.
In this study, an investigation was carried out into the occurrence of sulfamethoxazole (SMX) and trimethoprim (TMP) in the effluent of the university hospital (HUSM) of the UFSM. The degradation of these antimicrobials by the electrocoagulation (EC) process was also examined, in both the aqueous solution and hospital effluent, and a study was conducted in order to identify the subproducts formed. The experiments were optimized through factorial planning and, also, checked by response surface methodology. The best conditions for EC (achieving 58.0% of chemical oxygen demand (COD) reduction) were obtained by using 13 mA cm?2, 500 mg L?1 of NaCl, and 30 mm of interelectrode distance. The quantification of SMX (27.8 µg L?1) and TMP (6.65 µg L?1) in the hospital effluent, and the identification of the degradation products were carried out through liquid chromatography‐mass spectrometry quadrupole linear and ion trapping with electrospray ionization (LC‐ESI‐MS/MS_QTrap). Removals of 88.0% (degradation only) and 33.0% (adsorption only) were achieved for aqueous solutions of SMX and TMP, respectively, under optimized conditions. In hospital effluent samples, fortified with additions of SMX and TMP, corresponding removals of 16.0% (degradation) and 28.0% (adsorption) were achieved. This suggests that the EC process is efficient in degrading SMX in aqueous solution, although the same was not the case with TMP. The degradation products of SMX were identified (m/z 256.0 and 288.5); however, only the latter is mentioned in the literature. Toxicological aspects were not considered in this study.  相似文献   

18.
Wetlands often form the transition zone between upland soils and watershed streams, however, stream–wetland interactions and hydrobiogeochemical processes are poorly understood. We measured changes in stream nitrogen (N) through one riparian wetland and one beaver meadow in the Archer Creek watershed in the Adirondack Mountains of New York State, USA from 1 March to 31 July 1996. In the riparian wetland we also measured changes in groundwater N. Groundwater N changed significantly from tension lysimeters at the edge of the peatland to piezometer nests within the peatland. Mean N concentrations at the peatland perimeter were 1·5, 0·5 and 18·6 µmol L?1 for NH4+, NO3? and DON (dissolved organic nitrogen), respectively, whereas peatland groundwater N concentration was 56·9, 1·5 and 31·6 µmol L?1 for NH4+, NO3? and DON, respectively. The mean concentrations of stream water N species at the inlet to the wetlands were 1·5, 10·1 and 16·9 µmol L?1 for NH4+, NO3? and DON, respectively and 1·6, 28·1 and 8·4 µmol L?1 at the wetland outlet. Although groundwater total dissolved N (TDN) concentrations changed more than stream water TDN through the wetlands, hydrological cross‐sections for the peatland showed that wetland groundwater contributed minimally to stream flow during the study period. Therefore, surface water N chemistry was affected more by in‐stream N transformations than by groundwater N transformations because the in‐stream changes, although small, affected a much greater volume of water. Stream water N input–output budgets indicated that the riparian peatland retained 0·16 mol N ha?1 day?1 of total dissolved N and the beaver meadow retained 0·26 mol N ha?1 day?1 during the study period. Nitrate dominated surface water TDN flux from the wetlands during the spring whereas DON dominated during the summer. This study demonstrates that although groundwater N changed significantly in the riparian peatland, those changes were not reflected in the stream. Consequently, although in‐stream changes of N concentrations were less marked than those in groundwater, they had a greater effect on stream water chemistry—because wetland groundwater contributed minimally to stream flow. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

19.
Timber harvest temporarily increases water yield; however, relationships between hydrologic and nutrient chemistry changes have not been consistent. This study quantified the effects of forest harvesting and site preparation without fertilization and with modern best management practices on nutrient concentrations and yields in small headwater streams of the Southeastern Coastal Plain. We monitored two watershed pairs for 2 years prior to and 1 year following timber harvest and for 2 more years following site preparation and planting. Treatment watersheds were clearcut, and downstream portions of streamside management zones were thinned in Fall 2003. Site preparation (herbicide application and burning) and planting followed a year later. All operations followed 1999 Georgia forestry best management practices. Previously published research revealed a large increase in water yield following harvest. Nutrient concentrations varied significantly within and between monitoring periods, even in reference watersheds. Silvicultural activities had no discernible effect on phosphorus and ammonium concentrations; however, statistically significant increases in nitrate/nitrite (67–340 µg L−1) and total nitrogen concentrations (100–400 µg L−1) in treatment watersheds followed stand re‐establishment. Nutrient yields increased after timber harvest largely as a result of increased water yields, although increased nutrient yields were small relative to inter‐annual and inter‐watershed variability and variability. Annual water yield largely explained the variability in annual nitrogen and phosphorus export from reference and treatment streams (r2 values from 0.65 to 0.98). High NOx concentrations coming from an upstream agricultural area decreased 1600–1800 µg L−1 over several hundred metres in the treatment streams by dilution, uptake or denitrification. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

20.
Soil denitrification in reservoir shoreline wetlands is an important process for removing excess inorganic nitrogen from upland runoff and controlling eutrophication in aquatic ecosystems. As yet, little is known about the influence of vegetation characteristics on the soil denitrification potential in reservoir shoreline wetlands, although vegetation can affect both denitrifying bacteria and soil properties. In this study, we measured the spatial variability of denitrification enzyme activity (DEA) using acetylene block method in shoreline wetlands of the Danjiangkou Reservoir, a water source of the South‐to‐North Water Transfer Project in China. Results indicated that DEA ranged from 0.001 to 2.449 µg N (N2O) g?1 h?1, with a mean of 0.384 µg N (N2O) g?1 h?1. DEA varied significantly among five representative plant communities and the highest DEA (0.248–2.449 µg N (N2O) g?1 h?1) was observed in the Polygonum hydropiper community. Plant biomass and vegetation cover were significantly and positively related to DEA and together explained 44.2% of the total variance. These results suggest that vegetation characteristics should also be considered in assessing soil denitrification capacity and restoring shoreline wetlands for nitrogen pollution removal in the Danjiangkou Reservoir after dam heightening.  相似文献   

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