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1.
微波皂化萃取气相色谱法测定生物样品中的多氯联苯   总被引:3,自引:0,他引:3  
李攻科  何小青  杨云  张展霞 《分析化学》2000,28(9):1186-1186
1引言 多氯联苯(PCBs)的性质稳定、毒性大,贻贝等海洋生物能摄取和富集海水中的PCBs,因此研究其中PCBs的测定具有重要意义。生物样品中 PCBs的测定一般要进行预分离处理,索氏萃取分离 PCBs耗时至少8h,加碱皂化生物组织再以液-液萃取提取PCBs需要在沸水浴中回流1~2h,微波直接革取能有效地分离环境样品中的PCBs。本文利用微波皂化萃取(MASE)气相色谱法(GC)测定生物样品中的多氯联苯,实验以未受PCBs污染的淡水鱼为空白,用正交试验系统优化了微波功率、微波加热时间、皂化及萃取溶…  相似文献   

2.
非等间隔PCBs保留指数体系在光解行为研究中的应用   总被引:1,自引:0,他引:1  
苗秀生  储少岗  徐晓白 《色谱》1997,15(6):465-469
 利用Chu等已建立的多氯联苯(PCBs)非等间隔保留指数体系,由文献中的相对保留时间计算出全部209种PCBs同类物(Congener)的保留指数(IPCB)。利用IPCB结合GC-MS对PCB87、PCB138和PCB169三种同类物的光解产物进行了定性分析,发现其光解产物主要为低氯代联苯。实验结果证明,非等间隔保留指数体系IPCB在PCBs同类物的定性分析中具有准确、实用、快捷、方便等优点。  相似文献   

3.
将硒半胱氨酸(SeCysH)甲基化,对硒胱氨酸(SeCys)需还原后再甲基化。它们生成的甲基硒半胱氨酸(CH_3SeCysH)能与溴化氰(CNBr)发生专一性反应,定量生成的硒氰酸甲酯(CH_3SeN)可用气相色谱法(GC)测定。此法简称CNBr-GC法,检测限4×10 ̄(-8)克SeCys,准确度89.5%,相对标准差12.1%,非含硒氨基酸不干扰。此法适于样品中微量硒氨基酸(硒蛋氨酸SeMet,SeCysH和Secys)的测定。  相似文献   

4.
农晋琦  蔡端仁  欧阳政 《色谱》1994,12(1):28-31
 将硒半胱氨酸(SeCysH)甲基化,对硒胱氨酸(SeCys)需还原后再甲基化。它们生成的甲基硒半胱氨酸(CH_3SeCysH)能与溴化氰(CNBr)发生专一性反应,定量生成的硒氰酸甲酯(CH_3SeN)可用气相色谱法(GC)测定。此法简称CNBr-GC法,检测限4×10 ̄(-8)克SeCys,准确度89.5%,相对标准差12.1%,非含硒氨基酸不干扰。此法适于样品中微量硒氨基酸(硒蛋氨酸SeMet,SeCysH和Secys)的测定。  相似文献   

5.
建立了用GC-MS(SIM)内标定量法快速测定人尿中可待因及其代谢物浓度的方法,样品经酸水解、乙醚/异丙醇提取,用MSTFA-MBTFA衍生化后进样于GC-MSD,方法灵敏、准确,可用于监测吸毒者尿中可待因,吗啡类药物的浓度。本法已经受IOC的1992年水平考试的考验。  相似文献   

6.
建立了用GC-MS(SIM)内标定量法快速测定人尿中可待因及其代谢物浓度的方法。样品经酸水解、乙醚/异丙醇提取,用MSTFA-MBTFA衍生化后进样于GC-MSD,方法灵敏、准确,可用于监测吸毒者尿中可待因、吗啡类药物的浓度。本法已经受IOC的1992年水平考试的考验。  相似文献   

7.
SynthesisandCharacterizationofChiralLiquidCrystalCMPPCDPTIANYan-qing,ZHAOYing-ying,SUFeng-yuandTANGXin-yi(DepartmentofChemist...  相似文献   

8.
沙棘果皮水溶性多糖Hn的结构研究   总被引:22,自引:7,他引:15  
沙棘果皮水溶性多糖经酸性乙醇分级和DEAE-SephadexA-25sygg层析纯化,得到多糖Hn,经SepharoseCL-4B柱层析、玻璃纤维纸电泳、比旋光度测定等方法鉴定Hn为均一多糖。经唾液淀粉酶解、部分酸水解、高碘酸氧化、Smith降解、甲基化分析及IR,^13C-NMR,GC和GC-MS等方法,确定其基本结构中主链由1→4lc基,1→6Man基和1→6Gal基构成。三者摩尔比为nGlc  相似文献   

9.
用气相色谱-微波等离子体-原子发射光谱检测器(GC-MIP-AES)测定水中微量无机砷,在酸性条件下,As(Ⅲ与2,3-二巯基丙醇(BAL)的反应生成挥发性的环状二硫胂衍生物,被甲苯萃取,在181.379nm和189.041nm处GC-MIP-AES分别检测衍生物中硫砷的发射信号,检出限为15pg(以砷计)加标回收率96.35-106.03%,变异系数〈4.5%。  相似文献   

10.
SynthesisandStructureofSchiffBaseComplexContaining'Cu_4O'CoreMAChang-qin ̄*,YUZheng-gang,ZHANGWen-xing,WANGXu-ningandJIANGDe-h...  相似文献   

11.
A simple and rapid method based on pressurized liquid extraction has been validated for the simultaneous extraction of polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) from agricultural soil samples. Effective extraction was carried out in less than 17 min for all the studied compounds, and good recoveries were obtained for PAHs and PCBs, ranging from 70% to 112%, when blank samples were spiked at 2.5 μg kg−1, except for naphthalene with recoveries close to 40%. The separation and determination were performed by gas chromatography coupled to tandem mass spectrometry using a triple quadrupole mass analyzer. The target compounds were detected by electron impact with selected reaction monitoring, and mass spectrometric conditions were optimized in order to increase selectivity and sensitivity. The developed method was validated, and matrix-matched calibration was used for quantification purposes. Repeatability and interday precision ranged from 0.9% to 16.8% and from 1.6% to 22.3%, respectively. Limits of quantification ranged from 0.07 to 2.50 μg kg−1. The proposed method was applied to the analysis of agricultural soil samples collected from Almeria (Spain), and PAHs and PCBs were detected in some samples at concentrations ranging from 0.1 to 210 μg kg−1.  相似文献   

12.
Optimisation of microwave-assisted extraction (MAE) for the extraction of polychlorinated biphenyls (PCBs) from soil samples has been accomplished using an experimental design approach. Variables studied have been: percentage of acetone (v/v) in an acetone:n-hexane mixture, solvent volume, extraction time, microwave power and pressure inside the extraction vessel. Five samples of a certified soil (CRM 481) have been extracted under the optimum conditions of the developed method and the results have been compared to those obtained by Soxhlet extraction. Good recoveries (>95%) have been obtained for all the PCBs studied. All extracts have been analysed by gas chromatography/mass spectrometry (GC/MS) and an optimum determination method for the electron impact mass spectrometric (EIMS) has also been developed.  相似文献   

13.
Chlorobenzoic acids (CBAs) are the major metabolite of aerobic bacterial degradation of polychlorinated biphenyls (PCBs). A rapid and simple simultaneous derivatisation method has been developed for gas chromatography-mass spectrometry determination in historically PCB-contaminated soils for 15 isomers of mono-, di-, tri-, tetra-, and pentachlorobenzoic acids in CBA mixtures. Two derivatisation agents (diazomethane and methyl chloroformate) and various conditions were evaluated (temperature, time, solvents, catalysts) in terms of efficiency. The optimised derivatisation method with diazomethane and 1% methanol running 1 hour at 5°C was used for derivatisation of extracts of soils and river sediment from historically PCB-contaminated sites; the extracts were prepared using accelerated solvent extraction by a previously described method. Methylated CBAs were separated by gas chromatography using a system with two different common columns, DB-5 and DB-200, in series-coupled (tandem) arrangement and detected by EI-MS. A clean-up with a gel permeation chromatography was carried out to remove soil interfering matrix compounds as well as major portion of PCBs. The limits of quantification ranged between 1 and 10 ng g?1 of individual CBA in the soil. The procedure was applied to various soil samples from Lhenice (Czech Republic) highly contaminated with PCBs. CBAs were found in all tested soils and also in the river sediment. The most contaminated soil contained all CBAs representatives under the study with a total concentration of 3.1 µg g?1 of dry soil.  相似文献   

14.
A procedure focused on microwave-assisted extraction in open vessel (MAE-OV) and gas chromatography with electron capture detection (GC-ECD) was used for the determination of 26 congeners of polychlorinated biphenyls (PCBs) in soil samples. The limit of detection (LOD) and limit of quantification (LOQ) were evaluated for commercial PCBs mixture Aroclor1260. LOD and LOQ were calculated for each PCB congener, in the ranges (0.03–0.27?ng?g?1) and (0.11–0.70?ng?g?1), respectively. After optimization, 26 PCBs congeners were successfully extracted from soil samples with recovery amounts ranging between 84.7% and 117.3% for all PCBs congeners. The evaluated method of MAE-OV showed good separation and extraction of all PCBs congeners from soil samples. Extraction parameters such as solvent choice, power and extraction time were investigated. This study indicated that MAE-OV could be an interesting alternative method to extract PCBs from soils, since it is economical, easy, fast and requires low amounts of solvents.  相似文献   

15.
A novel method based on ultrasonic solvent extraction and stir bar sorptive extraction (SBSE) for the analysis of 51 persistent organic pollutants including organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and polybrominated diphenylethers (PBDEs) in soil samples was developed. The different parameters that affect both the extraction of analytes from the soil samples, such as solvent selection, solvent volume, mass of soil, and extraction time, and the partitioning from the solvent/water mixture to the PDMS were studied. The final selected conditions consisted of the extraction of 1 g of soil with 15 mL methanol by sonication for 30 min. The methanol extract was mixed with 85 mL of Milli-Q water and extracted by means of SBSE for 14 h at 900 rpm. The stir bars were analyzed by thermal desorption-GC-mass spectometry (TD-GC-MS). The effects of the matrix on the recovery of the various pollutants under the developed method were studied using two soils with very different physicochemical properties. Method sensitivity, linearity, repeatability, and reproducibility were also studied. Validation and accuracy of the method were conducted by analyzing two commercial certified reference materials (CRMs). The main advantage of this method resides in the fact that a small amount of a nontoxic solvent (methanol) is needed for the extraction of only 1 g of solid sample allowing LODs ranging from 0.01 to 2.0 microg/kg. Repeatability and reproducibility variations were lower than 20% for all investigated compounds. Results of the CRMs verify the high accuracy of this method.  相似文献   

16.
Several investigations on the extraction of dioxins from soil and fly ash with supercritical fluid have been reported; however, few of them describe the influence of components on the extraction. We extracted dioxins from eight samples with different values of organic carbon content and surface area with supercritical CO(2) at a temperature of 463 K, a pressure of 40 MPa, and using 10% toluene as an entrainer. We researched the influence of the characteristics of soil and fly ash on supercritical CO(2) extraction of dioxins. The results revealed that the extraction efficiencies of PCDD/DFs and PCBs were high for all soil samples, while that of fly ash samples decreased with the increase in organic carbon content and surface area. The extraction efficiencies of dioxins from four standard samples, activated carbon, humic acid, alumina, and florisil, were also examined. The results revealed that the extraction efficiencies were strongly influenced by activated carbon like components present in the samples.  相似文献   

17.
Abstract

Retrospective analysis of archived soil samples collected and stored from long-term agricultural experiments in the UK has shown how soil organic chemical composition has changed over time. High molecular weight polycyclic aromatic hydrocarbons (e.g. benzo[a]pyrene) and polychlorinated dibenzo-p-dioxins and -furans have increased in concentration through this century as a result of cumulative atmospheric depositional inputs. Concentrations of polychlorinated biphenyls and low molecular weight hydrocarbons (e.g. phenanthrene) peaked in the late 1960s/early 1970s, but have declined subsequently. This reflects declining atmospheric inputs of these compounds and losses from surface soils by volatilisation back to the atmosphere and biodegradation. PCBs and low molecular weight PAHs exist predominantly in the vapour phase in air, whilst heavy PAHs and PCDD/Fs are predominantly particulate-bound. Outgassing from soils is probably the most important contemporary source of PCBs to the atmosphere in the UK. Future UK PCB air concentrations will presumably therefore be influenced (controlled) by the rate of desorption and outgassing, as soil and air concentrations move towards a condition of equilibrium partitioning. Archived soils collected and stored before the commercial manufacture of PCBs contain no PCBs indicating that there is no ‘natural production’ of these compounds. However, within a few hours of exposure to contemporary air these samples contain detectable quantities of PCBs. Short-term air-soil exchange, such as during soil drying in the laboratory, can lead to contamination of samples which contain low concentrations of PCBs and loss from samples which contain high concentrations.  相似文献   

18.
Levels and patterns of polychlorinated biphenyls (PCBs) were studied in surface soil samples collected in the coastal part of Croatia within and surrounding four different airports and in the vicinity of two partially devastated electrical transformer stations. The compounds accumulated from air-dried soil samples by multiple ultrasonic extraction with an n-hexane?:?acetone 1?:?1 mixture were analysed by capillary gas chromatography with electron capture and ion-trap detection. PCBs were quantified against a standard Aroclor 1242/Aroclor 1260 mixture and a standard mixture of 17 individual PCB congeners (IUPAC No.: 28, 52, 60, 74, 101, 105, 114, 118, 123, 138, 153, 156, 157, 167, 170, 180, and 189). The mass fractions of total PCBs in 18 soil samples collected within the airport premises ranged from 3 to 41?327?µg/kg dry weight (dw) (median: 533?µg/kg?dw), and those in 21 samples collected at a distance ranging from several metres to 5?km away from the airport fence, from <1 to 39?µg/kg?dw (median: 5?µg/kg?dw). The highest PCB levels were determined in soils along the airport aprons where the aircrafts were serviced and refuelled. The PCB pattern was very similar to technical Aroclor 1260 in all airport soils. The PCB pattern in 22 soils collected in the vicinity of electrical transformer stations was dominated by congeners contained in Aroclor 1242. These soils contained 7 to >400?µg/kg?dw of total PCBs. One highly PCB-contaminated airport soil sample was analysed for polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs). With an international toxic equivalent (I-TEQ) of 9.7?ng/kg?dw, the airport soil contamination was within values typical for urban and rural areas, and the congener patterns gave no clear indication for PCBs as the only source of PCDDs/PCDFs.  相似文献   

19.
Polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs), such as DDT and analogues, hexachlorocyclohexane (HCH) isomers and hexachlorobenzene (HCB), were measured in surface soils and sediments from Eastern Romania. Thirty-nine soil samples from the forested zone, eight soil samples from a municipal waste-disposal site, and 10 sediment samples from the Bahlui River along the Iassy city were analysed using accelerated solvent extraction (ASE) and gas chromatography coupled to electron capture detection or mass spectrometry. The low mean concentrations of OCPs (11–31 and 22–84?ng?g?1 for HCHs and DDTs, respectively) and PCBs (8–43?ng?g?1) in soil samples from the forested zone suggest that contamination at most of these sites occurred predominantly through atmospheric transport from zones where these compounds were used and subsequently through atmospheric deposition. Contrarily, soil samples collected in the vicinity of a waste-disposal site near Iassy contained higher mean levels of PCBs (278?ng?g?1, range 34–1132?ng?g?1) than OCPs (6 and 101?ng?g?1 of soil for HCHs and DDTs, respectively). The sediment samples collected along the Bahlui river throughout the Iassy city revealed higher mean levels of PCBs (59?ng?g?1, range 24–158?ng?g?1) compared with OCP levels (2 and 37?ng?g?1 of soil for HCHs and DDTs, respectively). Furthermore, PCB profiles and concentrations in the sediment samples varied considerably along the river due to a wide variety of sources, such as different industries and waste sites. Although their sources are difficult to evaluate, the presence of POPs at most sites (especially at the waste-disposal site) may constitute a potential health hazard.  相似文献   

20.
A method was developed for viable and rapid determination of seven polychlorinated biphenyls (PCBs) in water samples with vortex-assisted liquid-liquid microextraction (VALLME) using gas chromatography-mass spectrometry (GC-MS). At first, the most suitable extraction solvent and extraction solvent volume were determined. Later, the parameters affecting the extraction efficiency such as vortex extraction time, rotational speed of the vortex, and ionic strength of the sample were optimized by using a 2(3) factorial experimental design. The optimized extraction conditions for 5 mL water sample were as follows: extractant solvent 200 μL of chloroform; vortex extraction time of 2 min at 3000 rpm; centrifugation 5 min at 4000 rpm, and no ionic strength. Under the optimum condition, limits of detection (LOD) ranged from 0.36 to 0.73 ng/L. Mean recoveries of PCBs from fortified water samples are 96% for three different fortification levels and RSDs of the recoveries are below 5%. The developed procedure was successfully applied to the determination of PCBs in real water and wastewater samples such as tap, well, surface, bottled waters, and municipal, treated municipal, and industrial wastewaters. The performance of the proposed method was compared with traditional liquid-liquid extraction (LLE) of real water samples and the results show that efficiency of proposed method is comparable to the LLE. However, the proposed method offers several advantages, i.e. reducing sample requirement for measurement of target compounds, less solvent consumption, and reducing the costs associated with solvent purchase and waste disposal. It is also viable, rapid, and easy to use for the analyses of PCBs in water samples by using GC-MS.  相似文献   

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