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961.
限进介质固相萃取及其应用 总被引:5,自引:0,他引:5
系统地介绍了限进介质固相萃取的原理、特点、发展现状及其发展趋势,并对该技术在生物和环境样品前处理中的应用作了较详细的综述。引用文献58篇。 相似文献
962.
963.
基于小波变换的高斯点扩展函数估计 总被引:16,自引:0,他引:16
点扩展函数估计是图像复原的重要内容,目前还没有精确估计的算法。根据小波理论,提出了新的高斯型点扩展函数精确估计算法。算法首先对模糊图像作平滑处理,抑止噪声;然后对图像进行不同尺度小波变换,并分别计算出变换后小波模极大值;再根据推导出的不同尺度下小波模极大值、李氏指数、方差三者之间的关系,准确计算出高斯点扩展函数的方差。实验结果表明,算法的估计精度高,达到了95%左右,具有重要的应用价值。 相似文献
964.
965.
分散液相微萃取-气相色谱/质谱快速分析水中的硝基苯类化合物 总被引:4,自引:1,他引:3
建立了分散液相微萃取.气相色谱,质谱快速分析水中硝基苯、对硝基苯、1,3一二硝基苯和2,4-二硝基氯苯的新方法.将含有18μL氯苯(萃取荆)的0.25 mL丙酮(分散剂)作为萃取体系,快速注入到5.0 mL水溶液中.在4000r/min下离心2.0 min后,得到(10.0±0.5)μL沉积相(氯苯),取底部沉积相1.0μL进行气相色谱,质谱分析.方法线性范围0.5~50μg/L(r2=0.9986~0.9994),检出限0.2~0.5μg/L,相对标准偏差4.2%~7.3%(n=5).将该方法用于环境水样的测定,加标回收率72.9%~89.6%. 相似文献
966.
分子印迹固相萃取-液相色谱质谱联用对4种磺酰脲类除草剂残留的测定 总被引:4,自引:2,他引:2
采用苄嘧磺隆分子印迹固相萃取柱(MISPE)对加标大米中的苄嘧磺隆、甲磺隆、苯磺隆和烟嘧磺隆4种磺酰脲类除草剂进行净化和富集预处理,并采用LC-MS方法进行定量分析.质谱条件为:正离子检测模式(M+H),检测质量范围为m/z 200 ~800 ,毛细管电压3.93 kV,锥孔电压20 V,脱溶剂温度250 ℃,辅助气流速4 L/min.4种磺酰脲类除草剂在0.01 ~0.70 mg·L~(-1)范围内线性良好.回收率为68% ~100%,表明样品液中的烟嘧磺隆、甲磺隆、苯磺隆和苄嘧磺隆能直接被分子印迹固相萃取柱中的印迹位点保留,而杂质几乎不被保留.分子印迹固相萃取柱对磺酰脲类除草剂表现出良好的识别性能. 相似文献
967.
A new method of hollow fiber liquid phase microextraction (HF-LPME) using ammonium pyrrolidine dithiocarbamate (APDC) as extractant combined with electrothermal atomic absorption spectrometry (ETAAS) using Pd as permanent modifier has been described for the speciation of As(III) and As(V). In a pH range of 3.0-4.0, the complex of As(III)-APDC complex can be extracted using toluene as the extraction solvent leaving As(V) in the aqueous layer. The post extraction organic phase was directly injected into ETAAS for the determination of As(III). To determine total arsenic in the samples, first As(V) was reduced to As(III) by l-cysteine, and then a microextraction method was performed prior to the determination of total arsenic. As(V) assay was based on subtracting As(III) form the total arsenic. All parameters, such as pH of solution, type of organic solvent, the amount of APDC, stirring rate and extraction time, affecting the separation of As(III) from As(V) and the extraction efficiency of As(III) were investigated, and the optimized extraction conditions were established. Under optimized conditions, a detection limit of 0.12 ng mL−1 with enrichment factor of 78 was achieved. The relative standard deviation (R.S.D.) of the method for five replicate determinations of 5 ng mL−1 As(III) was 8%. The developed method was applied to the speciation of As(III) and As(V) in fresh water and human hair extracts, and the recoveries for the spiked samples are 86-109%. In order to validate the developed method, three certified reference materials such as GBW07601 human hair, BW3209 and BW3210 environmental water were analyzed, and the results obtained were in good agreement with the certified values provided. 相似文献
968.
Xiujuan Liu Jianwang Li Zhixu Zhao Wei Zhang Kuangfei Lin Changjiang Huang Xuedong Wang 《Journal of chromatography. A》2009,1216(12):2220-2226
An analytical method, solid-phase extraction combined with dispersive liquid–liquid microextration (SPE–DLLME), was established to determine polybrominated diphenyl ethers (PBDEs) in water and plant samples. After concentration and purification of the samples in LC-C18 column, 1.0-mL elution sample containing 22.0 μL 1,1,2,2-tetrachloroethane was injected rapidly into the 5.0-mL pure water. After extraction and centrifuging, the sedimented phase was injected rapidly into gas chromatography with electron-capture detection (GC–ECD). For water samples, enrichment factors (EFs) are in the range of 6838–9405 under the optimum conditions. The calibration curves are linear in the range of 0.1–100 ng L−1 (BDEs 28, 47) and 0.5–500 ng L−1 (BDEs 100, 99, 85, 154, 153). The relative standard deviations (RSDs) and the limits of detection (LODs) are in the range of 4.2–7.9% (n = 5) and 0.03–0.15 ng L−1, respectively. For plant samples, RSDs and LODs are in the range of 5.9–11.3% and 0.04–0.16 μg kg−1, respectively. The relative recoveries of well, river, sea, leachate, and clover samples, spiked with different levels of PBDEs, are 66.8–94.1%, 72.2–100.5%, 74.5–110.4%, 62.1–105.1%, 66.1–91.7%, 62.4–88.9%, and 64.5–83.2%, respectively. The results show that SPE–DLLME is a suitable method for the determination of PBDEs in water and plant samples. 相似文献
969.
Dispersive liquid–liquid microextraction with little solvent consumption (DLLME-LSC), a novel dispersive liquid–liquid microextraction (DLLME) technique with few solvent requirements (13 μL of a binary mixture of disperser solvent and extraction solvent in the ratio of 6:4) and short extraction time (90 s), has been developed for extraction of organochlorine pesticides (OCPs) from water samples prior to gas chromatography/mass spectrometry analysis. In DLLME-LSC, much less volume of organic solvent is used as compared to DLLME. The new technique is less harmful to environment and yields a higher enrichment factor (1885–2648-fold in this study). Fine organic droplets were formed in the sample solution by manually shaking the test tube containing the mixture of sample solution and extraction solvent. The large surface area of the organic solvent droplets increases the rate of mass transfer from the water sample to the extractant and produces efficient extraction in a short period of time. DLLME-LSC shows good repeatability (RSD: 4.1–9.7% for reservoir water; 5.6–8.9% for river water) and high sensitivity (limits of detection: 0.8–2.5 ng/L for reservoir water; 0.4–1.3 ng/L for river water). The method can be used on various water samples (river water, tap water, sea water and reservoir water). It can be used for routine work for the investigation of OCPs. 相似文献
970.
A novel sample preparation method “Dispersive liquid–liquid–liquid microextraction” (DLLLME) was developed in this study. DLLLME was combined with liquid chromatography system to determine chlorophenoxy acid herbicide in aqueous samples. DLLLME is a rapid and environmentally friendly sample pretreatment method. In this study, 25 μL of 1,1,2,2-tetrachloroethane was added to the sample solution and the targeted analytes were extracted from the donor phase by manually shaking for 90 s. The organic phase was separated from the donor phase by centrifugation and was transferred into an insert. Acceptor phase was added to this insert. The analytes were then back-extracted into the acceptor phase by mixing the organic and acceptor phases by pumping those two solutions with a syringe plunger. After centrifugation, the organic phase was settled and removed with a microsyringe. The acceptor phase was injected into the UPLC system by auto sampler. Fine droplets were formed by shaking and pumping with the syringe plunger in DLLLME. The large interfacial area provided good extraction efficiency and shortened the extraction time needed. Conventional LLLME requires an extraction time of 40–60 min; an extraction time of approximately 2 min is sufficient with DLLLME. The DLLLME technique shows good linearity (r2 ≥ 0.999), good repeatability (RSD: 4.0–12.2% for tap water; 5.7–8.5% for river water) and high sensitivity (LODs: 0.10–0.60 μg/L for tap water; 0.11–0.95 μg/L for river water). 相似文献