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1.
建立了采用超声辅助分散液液微萃取技术结合高效液相色谱法(UA-DLLME-HPLC)对4种邻苯二甲酸酯(PAEs)进行富集、检测的方法,并成功应用于实际水样分析。实验中采用富集因子来评价萃取效率,考察并优化了影响萃取效率的主要因素,包括萃取剂类型和用量、分散剂类型和用量、超声时间、离子强度、萃取时间和pH值等。结果表明: 在最佳萃取条件下,该法对4种PAEs(邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯和邻苯二甲酸二正辛酯)具有较高的富集能力,富集因子分别为71、144、169和159;检出限分别为3.78、1.77、3.07和3.30 μg/L。对实验室自来水、某品牌矿泉水以及湖水分别加标50、200及500 μg/L的回收率为82.99%~114.47%,相对标准偏差为1.93%~8.31%。该法简便、快速、环保,可以用于测定实际水样中的PAEs类增塑剂。  相似文献   

2.
A new method was developed for simultaneous determination of five phthalate esters by a combination of mat-based solid-phase extraction (SPE) with high-performance liquid chromatography. The mat is composed of Nylon6 nanofibers. Dimethyl phthalate (DMP), diethl phthalate (DEP), di-n-butyl phthalate (DBP), di-(2-ethylhexyl) phthalate (DEHP) and dioctyl phthalate (DOP) were successfully separated on a RP-C18 column. Under optimized conditions, the detection limits found for DMP, DEP, DBP, DEHP and DOP were 3, 2, 6, 10 and 33 pg mL?1, respectively. The method was applied to the analysis of various water samples. Spiked samples gave recoveries in the range from 86.9 to 101.9%, with relative standard deviations below 7.0%. A comparison of Nylon6 nanofibers mat as sorbents, and C18 cartridges and other kinds of SPE sorbents was carried out with respect to recovery, sensitivity, and reproducibility. The results indicated that the Nylon mat is a viable material for the enrichment and determination of phthalate esters in environmental water samples.  相似文献   

3.
Phthalates (endocrine disrupters) released from food-contacted plastics into aqueous solution during microwave conditioning were measured with microdialysis enrichment on-lined high-performance liquid chromatography. The released phthalates in aqueous solution were diffused through a cellular dialysis membrane into the perfusion stream and thus enriched prior to HPLC analysis. Conditions for obtaining optimum enrichment such as the hollow dialysis fiber, flow-rate and polarity modifier in perfusion stream, pH, added-salt and stirring rate in sample solution, as well as chromatographic conditions were investigated. Experimental results indicated that microdialysis enrichment with a 20-cm polysulfone hollow dialysis fiber and heptane as the perfusate at 0.10-microL/min flow-rate to collect phthalates from aqueous sample in 0.5M KCl matrix (optional pH) at 250 rpm stirring offered the optimum enriched efficiency. The dimethyl phthalate (DMP), diethyl phthalate (DEP) and dibutyl phthalate (DBP) were well separated within 16 min by a C-18 column and eluted gradient from 40 to 90% aqueous acetonitrile (at pH 6.0) and 1.0 to 1.5 mL/min flow-rate. Detection was carried out with an UV detector at 225 nm. The enrichment factors were 14, 140 and 201 (at 0.10-microL/min perfusate flow-rate) for DMP, DEP and DBP, respectively, with less than 4% RSD. The proposed method provided a very simple, fast and eco-friendly enriched procedure to determine the extent of phthalates migration from disposable plastic materials into drinking soup.  相似文献   

4.
Pei Liang  Qian Li  Jing Xu  Dan Du 《Chromatographia》2008,68(5-6):393-397
A novel method, continuous-flow microextraction (CFME) combined with liquid chromatography (LC) with variable-wavelength detector (VWD), has been developed for the determination of three phthalate esters (dimethyl phthalate (DMP), diethyl phthalate (DEP), and di-n-butyl phthalate (DnBP)) in water samples. Experimental parameters including extraction solvent, solvent drop volume, flow rate of sample solution, extraction time and ionic strength, which affected the extraction efficiency, were studied and optimized. Under the optimum extraction conditions, the method yields a linear calibration curve in the concentration range of 10–10,000 ng mL?1 for target analytes. The enrichment factors of this method for DMP, DEP and DnBP reached at 27, 44 and 20, respectively, and the detection limits were 2, 1 and 5 ng mL?1, respectively. Good repeatability of extraction was obtained with relative standard deviations below 8.6%. The results demonstrated that CFME followed by LC-VWD is a simple and reliable technique for the determination of phthalate esters in water samples.  相似文献   

5.
A simple and sensitive method for the extraction of four phthalate esters including dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP) and di-n-butyl phthalate (DBP) as well as their determination in water samples was developed using homogeneous liquid–liquid extraction (HLLE) and HPLC-UV. The extraction method is based on the phase separation phenomenon by the salt addition to the ternary solvent system. The extraction parameters such as type and volume of extracting and consolute solvent, concentration of salt, pH of sample and extraction time were optimized. Under the optimal conditions (extraction solvent: 100?µL CHCl3; consolute solvent: 2.0?mL methanol; NaCl 15% (w/v) and pH of sample: 6.5) extraction recovery was in the range of 92–102%. Linearity was observed in the range of 0.5–300?µg?L?1 for DEP and 0.6–300?µg?L?1 for DMP, BBP and DBP. Correlation coefficients (r 2), limits of detection (LODs) and relative standard deviations (RSDs) were in the ranges of 0.9976–0.9993, 0.18–0.25 and 1.5–4.8%, respectively. The method was successfully applied for the preconcentration and determination of these phthalate esters in the several environmental water samples.  相似文献   

6.
高洁  杨偲  叶长文  李秀娟 《色谱》2009,27(3):356-358
选用自制杯[6]芳烃溶胶-凝胶固相微萃取(SPME)萃取头,建立了顶空SPME与气相色谱联用检测啤酒中8种酞酸酯(PAEs)的方法。采用L25(56)正交设计对萃取条件进行了优化,所得方法检出限为0.003~3.429 μg/L,相对标准偏差不超过13.5%,加标回收率为86.3%~109.3%。采用标准加入法对3种瓶装啤酒中PAEs进行了检测,结果表明邻苯二甲酸二(2-乙基己)酯(DEHP)是啤酒中最主要的酞酸酯类污染物,含量最高达5.24 μg/L。迁移试验表明,瓶装啤酒所用塑料垫圈中高含量的DEHP可能成为酒体中PAEs的一种来源,且延长贮存时间、提高贮存温度和振荡都能加快垫圈中DEHP的迁移。  相似文献   

7.
Yao J  Xu H  Lv L  Song D  Cui Y  Zhang T  Feng YQ 《Analytica chimica acta》2008,616(1):42-48
A novel liquid-phase microextraction (LPME) method was presented in this paper. The most attractive feature of this method is using a polychloroprene rubber tube (PCR tube) instead of a microsyringe to load organic solvent. The PCR tube and sample vial were horizontally placed so that the selection of organic solvent was not affected by the density of extractant. Therefore, the stability of organic solvent increased and the available organic solvent was extended greatly. In this work, three phthalate esters (PAEs) (dimethyl phthalate (DMP), diethyl phthalate (DEP), and di-n-butyl phthalate (DnBP)) were chosen as model analytes to testify the feasibility of the new method. A series of extraction parameters have been investigated systematically. Under the optimized condition, the method showed linear response over four orders of magnitude, ranged from 0.005 mg L−1 to 50 mg L−1. The correlation coefficients (r) were better than 0.997 and the limits of detection (LOD) were 0.0012 mg L−1 for DMP, 0.0014 mg L−1 for DEP and 0.0022 mg L−1 for DnBP. Good reproducibility of extraction was acquired, the inter-day and intra-day relative standard deviation (R.S.D.) were below 7.9% and 7.4%, respectively. Recoveries that ranged from 82.7% to 116.9% were gained when the new method was used to determine three phthalate esters in landfill leachates. The enrichment factors were 5–26 for the three PAEs. The novel LPME is promising to be an alternative sample preparation method for extracting target analytes in complex sample matrices because of the simplicity, low cost and short sample preparation time.  相似文献   

8.
王丽霞  寇立娟  潘峰云  王明林 《分析化学》2007,35(11):1559-1564
采用基质固相分散-液相色谱-质谱法测定保护地蔬菜中邻苯二甲酸酯(PAEs)含量,并分析了蔬菜中PAEs污染状况,研究了水和洗涤液浸泡对蔬菜中PAEs的消除效果。蔬菜样品经弗罗里硅土和石墨化碳黑研磨均匀后,用乙酸乙酯淋洗净化,再用液相色谱/电喷雾质谱法测定。PAEs的添加回收率为82.7%~105.7%;RSD为1.7%~6.1%;检出限为邻苯二甲酸二甲酯(DMP):0.99ng;邻苯二甲酸二乙酯(DEP):0.75ng;邻苯二甲酸二丁酯(DBP):0.70ng;邻苯二甲酸二异辛酯(DEHP):1.9ng。本方法前处理简单,具有较高的准确度和灵敏度。黄瓜、番茄、西葫芦中4种PAEs总量分别为2.02、1.26、0.91mg/kg;洗涤实验结果表明,水和洗涤液浸泡可显著降低蔬菜中的PAEs含量。  相似文献   

9.
QuEChERS/高效液相色谱测定食品中17种邻苯二甲酸酯   总被引:3,自引:0,他引:3  
建立了同时检测食品中17种邻苯二甲酸酯类化合物的QuEChERS/高效液相色谱分析方法.样品经乙腈提取,采用含50 mg PSA和150 mg MgSO4填料的净化管进行净化,分析液经C18柱分离,乙腈-水为流动相梯度洗脱,流速1.0 mL/min,紫外检测波长224 nm.在优化色谱条件下,DINP在0.5~10 m...  相似文献   

10.
Nano‐structured self‐doped polythiophene (SPT) electrodeposited in the presence of fluorinated organic acid was applied as a thermally stable conductive polymer‐based solid‐phase microextraction (SPME) fiber candidate. Quantitative determination of trace levels of phthalate esters including dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), and diethylhexyl phthalate (DEHP) was carried out using this novel fiber, coupling with gas chromatography‐flame ionization detector (GC‐FID). The SPT coating was proved to be stable at high temperatures (~350°C) with a high extraction capacity and long lifetime (more than 60 times). Improved temperature resistance was obtained by the presence of sulfonated groups in the backbone of polymer. Thermal stability of novel SPT was superior to common polythiophene (synthesized in LiClO4). The extraction procedure was optimized by means of the Taguchi orthogonal array experimental design with an OA16 (45) matrix including extraction temperature, extraction time, salt concentration, stirring rate, and headspace volume. The good linearity was obtained for most compounds with correlation coefficients (R2) of between 0.993 and 0.995. The detection limits were lower than 0.12 ng/mL for dimethyl phthalate, DEP, dibutyl phthalate, and diethylhexyl phthalate. The method was successfully applied to the analysis of water samples with the recoveries from 90±1 to 107±1%.  相似文献   

11.
The US Environmental Protection Agency (EPA) and the European Union (EU) have set restrictive limits for priority carcinogenic polycyclic aromatic hydrocarbons (CPAHs) in surface waters (EPA 3.8 ng L(-1) and EU 2-100 ng L(-1)) in order to protect aquatic life and human health. Currently, methods meeting these sensitivity criteria are not suitable for routine analysis of CPAHs. Here, we present a simple, rapid and low-cost method for the routine monitorization of these pollutants in aquatic environments based on their extraction with coacervates of decanoic acid reverse micelles in the nano- and microscale, and determination by liquid chromatography-fluorimetry (LC-FL). The method involves the stirring of filtered aqueous samples (36 mL) with 4 mL of THF containing 70 mg of decanoic acid for 5 min, its centrifugation for 10 min and the analysis of 20 microL of the resulting coacervate containing the CPAHs by LC/FL. The method is robust, the extractions being independent on salt concentration (up to 1 M), temperature (up to 60 degrees C) and pH (below 4). Besides, the coacervate prevents the CPAHs from adsorption onto the surface of containers during sample storage. No clean-up steps are necessary and the method is matrix-independent. The quantification and detection limits of the method ranged between 0.4 and 3.5 ng L(-1) and 0.1 and 1 ng L(-1), respectively, for the seven priority CPAHs. The method has been successfully applied to the determination of these pollutants in raw and treated sewage from three mechanical-biological treatment plants, two rivers and a reservoir with frequent motorized recreational craft activities, all of them located in the South of Spain. Recoveries for spiked samples in the range 2-30 ng L(-1) were between 88 and 95% with relative standard deviations from 1 to 7%. CPAHs were present in wastewater influents at concentrations in the range 3.9-37 ng L(-1), while the treatment at the WWTPs studied reduced their concentration in their respective effluents in a percentage near 100%. Three CPAHs were present at quantifiable levels in Guadajoz river (1.8-6.6 ng L(-1)) and six in La Bre?a reservoir (1.39-4.8 ng L(-1)).  相似文献   

12.
Phthalic acid esters (PAEs) have a negative impact on living organisms in the environment, therefore, are among the group of Endocrine Disrupting Compounds (ECDs). Unfortunately, conventional methods used in municipal wastewater treatment plants (MWWTPs) are not designed to eliminate PAEs. For this reason, the development of cheap and simple but very effective techniques for the removal of such residues from wastewater is crucial. The main aim of this study was the evaluation of the removal of six selected PAEs: diethyl phthalate (DEP), di-n-octyl phthalate (DOP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), bis(2-ethylhexyl) phthalate (DEHP) and dimethyl phthalate (DMP), in real MWWTPs supported by constructed wetlands (MWWTP–CW system). For the first time, the possibility of using three new plants for this purpose, Cyperus papyrus (papyrus), Lysimachia nemorum (yellow pimpernel) and Euonymus europaeus (European spindle), has been presented. For determining the target PAEs in wastewater samples, a method of SPE (Solid-Phase Extraction)–GC–MS(SIM) was developed and validated, and for plant materials, a method of UAE (Ultrasound-Assisted Extraction)–SPE–GC–MS(SIM) was proposed. The obtained data showed that the application of the MWWTP–CW system allows a significant increase in the removal of DEP, DBP, BBP and DEHP from the wastewater stream. Euonymus europaeus was the most effective among the tested plant species for the uptake of analytes (8938 ng × g−1 dry weight), thus, this plant was found to be optimal for supporting conventional MWWTPs.  相似文献   

13.
This study demonstrates the potential of bamboo charcoal as a novel and inexpensive solid-phase microextraction (SPME) coating material for enrichment and determination of organic pollutants in water samples. Bamboo charcoal was prepared and used as a SPME coating material. Eleven phthalate esters (PAEs) were used as model analytes, and gas chromatography–mass spectrometry was used for separation and detection. Important extraction conditions (ionic strength, stirring rate, and extraction time) and desorption conditions (desorption temperature and time) were systematically investigated and optimized. Linearity of 0.1–100 μg?L?1 and correlation coefficients of 0.9992–0.9998 were obtained under optimum conditions. Inter-day and intra-day repeatability were 2.15–9.93 % and 1.89–9.85 %, respectively, and fiber-to-fiber reproducibility was 5.42–9.66 %. On the basis of a chromatographic signal-to-baseline noise ratio of three, the limits of detection reached 0.004–0.023 μg?L?1. Satisfactory results were achieved when the bamboo coating was used for determination of 11 PAEs in real water samples. The experimental results indicate that bamboo charcoal has significant potential as a SPME coating material for rapid enrichment and sensitive determination of organic pollutants in environmental samples.  相似文献   

14.
A fast and simple method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has been applied to identify and quantify four phthalic acid esters (PAEs) in different contact lens cleaning solutions. A migration study of these compounds from contact lenses has also been performed. The PAEs studied were dimethyl phthalate, diethyl phthalate, butyl benzyl phthalate and dibutyl phthalate. The migration of PAEs from contact lenses was performed by suspending each contact lens in an artificial tear solution at 37 °C and shaking it at 130 rpm for 24 h. The purpose of this study was to determine a possible migration of these compounds to the eyes as a result of the use of contact lenses and their cleaning solutions. The method was precise (with relative standard deviation (RSD) from 2.2 to 11.9%). It was also sensitive, with LODs of 0.03, 0.19, 0.31 and 2.62 μg L− 1 for DMP, DEP, BBP and DBP respectively. The results obtained confirm the presence of these substances in some types of contact lens cleaning solutions. Furthermore, DBP and BBP were liberated from the contact lenses during the migration study.  相似文献   

15.
A technique of ultrasound-assisted low density solvent based dispersive liquid-liquid microextraction was developed for the determination of four phthalate esters, including dimethyl phthalate(DMP), diethyl phthalate(DEP), di-n-butyl phthalate(DnBP) and di(2-ethylhexyl) phthalate(DEHP) in bottled water samples. A low density solvent, toluene, was selected as extraction solvent. In the extraction process, a mixture of 15 μL of toluene(extraction solvent) and 100 μL of methanol(disperser solvent) was rapidly injected into 1.0 mL of water samples. A cloudy solution was formed after ultrasounded for 5 min, and then centrifuged at 5000 r/min for 5 min. The enriched analytes in the floating phase were determined by means of gas chromatograph. Under the optimum conditions, the enrichment factors were found to be in a range of 29-67, and the recoveries were ranged from 81.2% to 103.9%. The limits of the detection were in a range of 3.8-5.6 μg/L. The proposed method was applied to the extraction and determination of phthalate esters in bottled water samples, and the concentrations of phthalate esters found in the water samples were below the allowable levels.  相似文献   

16.
李玫瑰  李元星  毛丽秋 《色谱》2007,25(1):35-38
将一种新型、简单、快速、环境友好的萃取方法微滴液相微萃取(SDME)与气相色谱-质谱法结合用于快速分析食品中的几种酞酸酯(PAEs)。考察了萃取溶剂的种类及用量、微液滴在样品溶液中的深度、萃取时间及搅拌子的搅拌速度对微滴液相微萃取的影响。优化的萃取条件为:萃取溶剂为2.0 μL甲苯,微液滴在样品溶液中的深度为0.75 cm,搅拌速度为1000 r/min,萃取时间为20 min。该方法的线性范围为0.1~4000 μg/L,检测限为25 ng/L~0.8 mg/L,加标回收率为87.1%~114.4%,相对标准偏差为4.9%~11.6%。微滴液相微萃取所需的有机溶剂量很小,是一种快速、简单、安全、有效的水溶性样品的前处理方法。  相似文献   

17.
A sensitive and selective column adsorption method is proposed for the off-line preconcentration and determination of phthalic acid esters (PAEs), namely benzyl-butyl phthalate (BBP), di-n-butyl phthalate (DBP) and di-cyclohexyl phthalate (DCHP). The PAEs was preconcentrated on Saccharomyces cerevisiae immobilized on silica gel and then determined by high performance liquid chromatography (HPLC). Several parameters on the recovery of the analytes were investigated. Recoveries of BBP, DBP and DCHP were 100±2, 98±2 and 98±3%, respectively, at 95% confidence level under optimum conditions. The detection limits (3S/N) of BBP, DBP and DCHP were 3.2, 6.3 and 3.1 μg l−1, respectively. The capacity of the adsorbent was also examined and found to be 1.4 mg g−1 for BBP and DBP, and 3.6 mg g−1 for DCHP. S. cerevisiae immobilized on silica gel is suitable for repeated use without decreasing recovery up to about 25 adsorption-elution cycles. The proposed method was successfully applied to the determination of PAEs in river water with high precision and accuracy.  相似文献   

18.
Six phthalate acid esters(PAEs) priority pollutants[dimethyl phthalate(DMP), diethyl phthalate(DEP), dibutyl phthalate (DBP or DNBP), di-n-octyl phthalate(DNOP), di 2-ethyl hexyl phthalate(DEHP), and butyl benzyl phthalate(BBP)] were opted as the research object. PAE-degrading esterase CarEW(PDB ID:1C7I) isolated from Bacillus subtilis acting as a template and an iterative saturation mutation strategy was adopted to modify key amino acids to attain efficient PAE-degrading esterase substitutes with a reasonable structure constructed by homology modeling method. Present study designed a total of 285 unit-site and multi-site substitutions of PAE-degrading esterase using the homology modeling method. Among them, 207 PAE-degrading esterase substitutions, which contained the 6-site PAE-degrading esterase substitute 1C7I-6-9 with 84.21% enhancement intensity of degradation ability revealed better degradability to all the 6 PAEs after modification. Moreover, molecular dynamics simulation based on the Taguchi method reported the optimal external application environment for PAE-degrading esterase substitutes as follows:pH=6, T=35℃, the rhamnolipid concentration was 50 mg/L, the molar ratio of nitrogen to phosphorus(N:P) was 10:1, the concentration of H2O2 was 50 mg/L, and the voltage gradient was 1.5 V/cm. The degradation ability of PAE-degrading esterase substitutes was found to be elevated by 13.04% as compared to that of the blank control under the optimal condition. Moreover, 11 highly efficient PAE-degrading esterase substitutes with thermal stability were designed.  相似文献   

19.
韦俊芳  姜磊  楼超艳  朱岩 《色谱》2018,36(7):678-684
建立了同时快速测定运动饮料中邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丙酯、邻苯二甲酸二丁酯、邻苯二甲酸二戊酯、邻苯二甲酸丁基苄基酯、邻苯二甲酸二(2-乙基己基)酯、邻苯二甲酸二辛酯8种邻苯二甲酸酯(PAEs)类增塑剂的超临界流体色谱-紫外检测分析方法。实际样品经液相萃取后,用超临界流体色谱分析,以超临界态二氧化碳-3%(体积分数)甲醇作为色谱流动相进行等度洗脱,检测波长为225 nm,6 min即可实现分离。8种PAE类增塑剂在0.05~25 mg/L范围内均具有良好的线性关系,相关系数为0.9991~0.9997,方法检出限为7.5~15 μg/L。8种PAE类增塑剂在运动饮料样品中的加标回收率为91.7%~100.2%,相对标准偏差均不大于6.5%(n=3)。应用该方法对多种市售运动饮料中的8种PAE类增塑剂进行检测,结果表明,该方法环保、快速、灵敏、选择性高、结果准确,能满足运动饮料中增塑剂含量检测的要求。  相似文献   

20.
采用胶束扫集毛细管电动色谱技术,建立了测定药物中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DZP)和邻苯二甲酸二丁酯(DBP)的方法。电泳缓冲体系含80 mmol/L SDS,20 mmol/L NaH2PO4(pH 2.20),5%甲醇(V/V),分离电压-18 kV,重力进样80s×15.0cm,检测波长225 nm,使用Φ50μm×62.0 cm石英毛细管,有效长度50.0 cm。讨论了磷酸盐浓度、有机改善剂、SDS浓度、分离电压、进样时间等因素的影响,并考察了胶束扫集法对DMP、DEP和DBP的富集能力。在优化条件下,线性关系良好,相关系数大于0.9986,DMP、DEP和DBP的线性范围分别为1.25~240,1.04~200和1.56~200 mg/L,检出限分别为0.26,0.26和0.39 mg/L。方法应用于肠溶片中DMP、DEP和DBP的测定,回收率在93.3%~108%之间,RSD≤5.2%。每次样品测定可在10 min内完成。  相似文献   

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