共查询到20条相似文献,搜索用时 15 毫秒
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WANG Qin-Sun ZHU Chang-Shou YAN Bing-WenNational Laboratory of Elemento-Organic Chemistry Nankai University Tianjin China 《中国化学》1995,(2)
A computer-assisted advanced simplex method is presented for the simultaneous optimization of multifactor ( stationary phase loading, carrier gas flow rate and column temperature ) for separation of ten compounds in gas chromatography. A three factors factorial design was used. The method was based on a special polynomial established from fifteen preliminary runs, using resolution as the selection criterion, with connection to a general simplex method. Excellent agreement is found between the predicted data and the experimental results, and most of experiments required in the general simplex method can be omitted. 相似文献
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Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, < 7%), correlation coefficient (> 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden. 相似文献
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Summary This paper describes a study of the potential of large-volume on-column injection for the determination of triazine herbicides
in clean water samples (ground-water). The sensitivity of chromatographic determination has been increased by two orders of
magnitude by injection of up to 200 μL of pesticide solutions and nitrogen-phosphorus detection. Analytical characteristics
expressed as precision, linear range and limit of detection have been determined, the results indicating adequate analytical
performance and the ruggedness of the injection technique. As an application, gas chromatography with large-volume on-column
injection and nitrogen-phosphorus detection was combined with off-line liquid-liquid micro-extraction with hexane (1 mL water/1
mL hexane). The procedure was applied to spiked groundwater samples at two concentration levels (1 and 10 μg L−1) with good recoveries (between 81 and 103%, except for deethylatrazine) and repeatability (better than 15% at the 1 μg L−1 level). Limits of detection of the triazine herbicides studied ranged from 0.08 to 0.16 μgL−1. 相似文献
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R F Adams 《Journal of chromatography. A》1974,95(2):189-212
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气相色谱法测定苹果和土壤中的高效氯氟氰菊酯 总被引:1,自引:0,他引:1
建立了改进的QuEChERS-气相色谱检测苹果和土壤中高效氯氟氰菊酯残留的分析方法,考察和评价了苹果和土壤两种基质对高效氯氟氰菊酯的基质效应。苹果和土壤样品均用乙腈提取,经石墨化碳黑(GCB)净化后直接进样分析。结果表明:在优化后的QuEChERS条件下,高效氯氟氰菊酯在0.05~10 mg/L范围内线性关系良好,相关系数(R2)大于0.999,检出限为0.12~0.15 μg/kg,定量限为0.38~0.50 μg/kg。用基质标准曲线定量时,高效氯氟氰菊酯在土壤和苹果中的回收率分别为88.29%~97.65%和80.70%~98.69%。苹果和土壤样品对高效氯氟氰菊酯都表现出基质增强效应。该方法的回收率均能达到残留分析要求,用基质配制标准溶液能够有效、方便地校正气相色谱-电子捕获检测器测定高效氯氟氰菊酯残留时的基质效应,且能应用于苹果和土壤实际样品的检测。 相似文献
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Determination of the chloroacetanilide herbicides in waters using single-drop microextraction and gas chromatography 总被引:2,自引:0,他引:2
Er-cheng Zhao Wei-li Shan Shu-ren Jiang Yu Liu Zhi-qiang Zhou 《Microchemical Journal》2006,83(2):105-110
In this article, a new method using single-drop microextraction (SDME) and gas chromatography micro-electron capture detection (GC-μECD) for the determination of chloroacetanilide herbicides (alachlor, acetochlor, metolachlor, pretilachlor and butachlor) residues was developed. The effects of SDME parameters such as extraction solvent, stirring rate, ionic strength, microdrop volume and extraction time were optimized. The optimum experimental conditions found were: 1.6 μl toluene microdrop, 5 ml water sample, 400 rpm stirring rate, 15 min extraction time and no salt addition. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The proposed method was proved to be a simple and rapid analytical procedure for chloroacetanilide herbicides in water with limits of detection 0.0002–0.114 μg/l. The relative recoveries range from 80% to 102% for all the target analytes, with the relative standard deviations varying from 3.9% to 11.7%. 相似文献
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顶空气相色谱法测定聚苯乙烯日用品中可溶性苯乙烯单体 总被引:1,自引:0,他引:1
应用带有顶空进样器气相色谱仪,采用外标法定量,分别以乙醇、乙醇 水作提取剂,分析了聚苯乙烯日用品中可溶性苯乙烯的含量,并对其提取温度、时间进行了研究。在选择的色谱条件下,用乙醇、乙醇 水提取苯乙烯标准溶液分别在0.8~5000mg L、0.1~200mg L浓度间呈现良好的线性关系,检出限<0.1mg L,其相对标准偏差分别为3.2%、5.9%。 相似文献
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Determination of triazine herbicides in human body fluids by solid-phase microextraction and capillary gas chromatography 总被引:2,自引:0,他引:2
T. Kumazawa X. -P. Lee K. Kondo K. Sato H. Seno K. Watanabe-Suzuki A. Ishii O. Suzuki 《Chromatographia》2000,52(3-4):195-199
Summary Eight triazine herbicides, prometon, propazine, atrazine, simazine, prometryn, ametryn, metribuzin, and cyanazine, have been
extracted from human whole blood and urine samples by headspace solid-phase microextraction (SPME) with a polydimethylsiloxane-coated
fiber and quantified by capillary gas chromatography with nitrogen-phosphorus detection.
Extraction efficiencies for all compounds were 0.21–0.99% for whole blood, except for cyanazine (0.06%). For urine, the extraction
efficiencies for prometon, propazine, atrazine, prometryn and ametryn were 13.6–38.1%, and those of simazine, metribuzin and
cyanazine were 1.35–8.73%.
The regression equations for the compounds extracted from whole blood were linear within the concentration ranged 0.01–1 μg
(0.5 mL)−1 for prometon, propazine, atrazine, prometryn, and ametryn, and 0.02–1 μg (0.5 mL)−1 for simazine, metribuzin, and cyanazine. For urine, regression equations for all compounds were linear within the concentration
range 0.005–0.25 μg mL−1. Compound detection limits were 2.8–9.0 ng (0.5 mL)−1 and 0.4–2.0 ng mL−1 for whole blood and urine, respectively. The coefficients of within-day and day-to-day variation were satisfactory for all
the compounds, and not greater than 10.3 and 14.2%, respectively.
Data obtained from determination of atrazine in rat whole blood after oral administration of the compound are also presented. 相似文献
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Summary A sensitive gas chromatographic method is described for the analysis of fosfomycin (FOS) in chicken plasma using phenylphosphonic
acid (PPA) as the internal standard. Plasma samples were ultrafiltered, and the ultrafiltrate was then evaporated to dryness.
The residue was reconstituted with a silylation reagent for the derivatization of FOS and PPA. The methodology involves the
use of a HP-5 capillary column and a flame ionisation detector (FID). The retention times of FOS and PPA were 4.63 and 8.68
minutes, respectively. Response was linear in the range of 1–150 μ mL−1. The detection and quantitation limits were 1 and 2.1 μ mL−1, respectively. Recovery was determined as 109% for FOS. The method was applied to the determination of FOS in chicken plasma
samples collected during pharmacokinetic studies. 相似文献
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Ultrasound-assisted emulsification microextraction was applied to extract the herbicides simazine, atrazine, prometon, ametryn and prometryn from soil samples. They then were determined by HPLC with diode-array detection. Parameters that affect the extraction efficiency, such as the kind and volume of the extraction solvent, emulsification time and addition of salt, were optimized. Under the optimum conditions, the following analytical figures of merits are found: enrichment factors between 145 and 222, limits of detection between 0.1 to 0.5 ng g?1, analytical linearity in the range from 1.0 to 200 ng g?1, correlation coefficients (r) between 0.9989 and 0.9998, relative standard deviations from 2.8% to 3.6% (at n?=?5, intraday) and 3.7% to 4.3% (interday), and recoveries (at spiking levels of 5.0 and 50.0 ng g?1) from 82.6% to 92.0%. The technique is simple, practical, rapid, and environmentally friendly. 相似文献
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Determination of Aroclor 1260 in soil samples by gas chromatography with mass spectrometry and solid‐phase microextraction 下载免费PDF全文
Mengliang Zhang Glen P. Jackson Natalie A. Kruse Jennifer R. Bowman Peter de B. Harrington 《Journal of separation science》2014,37(19):2751-2756
A novel fast screening method was developed for the determination of polychlorinated biphenyls that are constituents of the commercial mixture, Aroclor 1260, in soil matrices by gas chromatography with mass spectrometry combined with solid‐phase microextraction. Nonequilibrium headspace solid‐phase microextraction with a 100 μm polydimethylsiloxane fiber was used to extract polychlorinated biphenyls from 0.5 g of soil matrix. The use of 2 mL of saturated potassium dichromate in 6 M sulfuric acid solution improved the reproducibility of the extractions and the mass transfer of the polychlorinated biphenyls from the soil matrix to the microextraction fiber via the headspace. The extraction time was 30 min at 100°C. The percent recoveries, which were evaluated using an Aroclor 1260 standard and liquid injection, were within the range of 54.9–65.7%. Two‐way extracted ion chromatogram data were used to construct calibration curves. The relative error was <±15% and the relative standard deviation was <15%, which are respective measures of the accuracy and precision. The method was validated with certified soil samples and the predicted concentrations for Aroclor 1260 agreed with the certified values. The method was demonstrated to be linear from 10 to 1000 ng/g for Aroclor 1260 in dry soil. 相似文献
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Anizio M. Faria Raquel P. Dardengo Claudio F. Lima Antonio A. Neves 《International journal of environmental analytical chemistry》2013,93(4):249-258
This article proposes an alternative method, using cloud-point extraction and gas chromatography, for extraction and determination of disulfoton in water samples. For cloud-point extraction, the nonionic surfactant Triton X-114 was used. Before gas chromatography, a cleanup stage for surfactant removal from the extracts was optimized. Cleanup used two columns, in series, containing silica gel and Florisil, with methanol:hexane (1?:?1) as eluent, resulting in the removal of more than 95% of the Triton X-114. Factors such as ionic strength (>0.5?mol?L?1) and surfactant concentration (1.0% w/v) increased the extraction efficiency of the cloud-point methodology, yielding disulfoton recoveries of almost 100%. Compared with liquid–liquid extraction, the cloud-point methodology was more efficient, with a better detectability, and resulted in a significant reduction in solvent volume. 相似文献
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A simple, rapid, efficient, and environmentally friendly method for the determination of five triazine herbicides in water and soil samples was developed by using dispersive liquid-liquid microextraction (DLLME), coupled with high performance liquid chromatography-diode array detection (HPLC-DAD). The water samples were directly used for DLLME extraction. For soil samples, the target analytes were first extracted by water-methanol (99:1, v/v). In the DLLME extraction method, chloroform was used as an extraction solvent, and acetonitrile as a dispersive solvent. Under the optimum conditions, the enrichment factors of DLLME were in the range between 183-221. The linearity of the method was obtained in the range of 0.5-200 ng/mL for the water sample analysis, and 1-200 ng/g for the soil samples, respectively. The correlation coefficients ranged from 0.9968 to 0.9999. The limits of detection were 0.05-0.1 ng/mL for the water samples, and 0.1-0.2 ng/g for the soil samples. The proposed method has been successfully applied to the analysis of target triazine herbicides (simazin, atrazine, prometon, ametryn, and prometryn) in water and soil samples with satisfactory results. 相似文献
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The method presented uses reversed-phase liquid chromatography with negative electrospray ionization and tandem mass spectrometry to analyze 9 chlorinated acid herbicides in soil and vegetation matrixes: clopyralid, dicamba, MCPP, MCPA, 2,4-DP, 2,4-D, triclopyr, 2,4-DB, and picloram. A 20 g portion is extracted with a basic solution and an aliquot acidified and micropartitioned with 3 mL chloroform. Vegetation samples are subjected to an additional cleanup with a mixed-mode anion exchange solid-phase extraction cartridge. Two precursor product ion transitions per analyte are measured and evaluated to provide the maximum degree of confidence in results. Average recoveries for 3 different soil types tested ranged from 72 to 107% for all compounds with the exception of 2,4-DB at 56-99%. Average recoveries for the 3 different vegetation types studied were lower and ranged from 53 to 80% for all compounds. 相似文献
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A simple and rapid new dispersive liquid-liquid microextraction technique (DLLME) coupled with gas chromatography-ion trap mass spectrometric detection (GC-MS) was developed for the extraction and analysis of triazine herbicides from water samples. In this method, a mixture of 12.0 microL chlorobenzene (extraction solvent) and 1.00 mL acetone (disperser solvent) is rapidly injected by syringe into the 5.00 mL water sample containing 4% (w/v) sodium chloride. In this process, triazines in the water sample are extracted into the fine droplets of chlorobenzene. After centrifuging for 5 min at 6000 rpm, the fine droplets of chlorobenzene are sedimented in the bottom of the conical test tube (8.0+/-0.3 microL). The settled phase (2.0 microL) is collected and injected into the GC-MS for separation and determination of triazines. Some important parameters, viz, type of extraction solvent, identity and volume of disperser solvent, extraction time, and salt effect, which affect on DLLME were studied. Under optimum conditions the enrichment factors and extraction recoveries were high and ranged between 151-722 and 24.2-115.6%, respectively. The linear range was wide (0.2-200 microg L(-1)) and the limits of detection were between 0.021 and 0.12 microg L(-1) for most of the analytes. The relative standard deviations (RSDs) for 5.00 microg L(-1) of triazines in water were in the range of 1.36-8.67%. The performance of the method was checked by analysis of river and tap water samples, and the relative recoveries of triazines from river and tap water at a spiking level of 5.0 microg L(-1) were 85.2-114.5% and 87.8-119.4%, respectively. This method was also compared with solid-phase microextraction (SPME) and hollow fiber protected liquid-phase microextraction (HFP-LPME) methods. DLLME is a very simple and rapid method, requiring less than 3 min. It also has high enrichment factors and recoveries for the extraction of triazines from water. 相似文献
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微波辅助萃取-气相色谱测定土壤中多氯联苯 总被引:2,自引:0,他引:2
建立了微波辅助萃取-气相色谱-微电子捕获检测土壤样品中6种多氯联苯(pcb28, pcb52, pcb101, pcb138, pcb153和pcb180)的方法. 确定了以V(20 mL丙酮):V(正己烷)=1:1混合溶剂作萃取剂, 萃取温度110 ℃, 仪器功率800 W, 微波萃取5 min的样品前处理条件, 并用柱温程序优化了GC-μECD分析条件. 方法的检出限为0.027~0.087 ng/g; 相对标准偏差为3.4%~7.6% (n=6); 加标平均回收率79.8%~91.1%. 可用于土壤环境中多氯联苯的监测分析. 相似文献