饮用水中有机污染物检测方法研究进展

介绍水中有机污染物的富集方法如顶空法、萃取法、固相微萃取法、液相微萃取法、棒吸附萃取等,对饮用水中有机污染物的检测技术如气相色谱法、气相色谱–质谱联用法、液相色谱法、液相色谱–质联用法等进行了综述并对检测技术的发展趋势进行了展望。     

冷冻干燥技术在环境水样有机新污染物前处理中的应用进展

有机新污染物是一类在先进分析技术帮助下新鉴定的、现有法规未管制的、人为源的有机污染物.有机新污染物主要包括药品与个人护理、农药、全氟化合物、内分泌干扰物等,其会产生内分泌干扰效应、诱发抗性基因传播,还对人类和野生生物的生存与发展构成潜在威胁,因此检测环境样品中的有机新污染物浓度对生态环境和人体健康具有重大意义.由于环境...     

金属有机框架材料MIL-101在吸附去除水中有机污染物中的应用进展

金属有机框架材料（MOFs）是一种极具前景的水中污染物吸附材料,其中,拉瓦锡研究所材料（MIL）凭借较好的稳定性和较多的可调节位点在众多MOFs中脱颖而出。与其他MILs相比,MIL-101具有比表面积较大和表面活性位点多的特点,在水中的稳定性高,已成为一种新兴的吸附材料。鉴于此,该文对近年来MIL-101在水中有机污染物去除领域的应用研究进行了综述,主要对MIL-101结构、改性修饰及其在水污染物吸附去除方面的应用及吸附机理进行了介绍。最后对MIL-101吸附材料的应用前景进行了分析和展望。     

固相萃取-气相色谱/质谱选择离子检测法测定水中27种有机农药EI北大核心CSCD

采用固相萃取(SPE)技术,结合气相色谱/质谱(GC-MS)选择离子检测法(SIM)对水中27种有机农药进行提取、净化、浓缩前处理,实验优选出了分离效果较好的色谱柱VF-1701 ms(30 m×0.25 mm×0.25μm),优化了固相萃取及GC-MS的分析条件,建立了水样中7类27种有机农药的SPE-GC-MS/SIM分析方法。样品中各组分曲线相关系数R2均大于0.9981,检测限为0.015~0.054μg/L,平均加标回收率为72.8%~110.8%,相对标准偏差RSD为5.5%~16%。与传统方法相比,该法无需对有机污染物进行分类处理,可以同时快速测定7类27种有机农药。     

固相萃取-气相色谱/质谱选择离子检测法测定水中27种有机农药EI北大核心CSCD

采用固相萃取(SPE)技术,结合气相色谱/质谱(GC-MS)选择离子检测法(SIM)对水中27种有机农药进行提取、净化、浓缩前处理,实验优选出了分离效果较好的色谱柱VF-1701 ms(30 m×0.25 mm×0.25μm),优化了固相萃取及GC-MS的分析条件,建立了水样中7类27种有机农药的SPE-GC-MS/SIM分析方法。样品中各组分曲线相关系数R2均大于0.9981,检测限为0.015~0.054μg/L,平均加标回收率为72.8%~110.8%,相对标准偏差RSD为5.5%~16%。与传统方法相比,该法无需对有机污染物进行分类处理,可以同时快速测定7类27种有机农药。     

固相萃取-气相色谱/质谱选择离子检测法测定水中27种有机农药

采用固相萃取(SPE)技术,结合气相色谱/质谱(GC-MS)选择离子检测法(SIM)对水中27种有机农药进行提取、净化、浓缩前处理,实验优选出了分离效果较好的色谱柱VF-1701 ms(30 m×0.25 mm×0.25μm),优化了固相萃取及GC-MS的分析条件,建立了水样中7类27种有机农药的SPE-GC-MS/SIM分析方法。样品中各组分曲线相关系数R2均大于0.9981,检测限为0.015~0.054μg/L,平均加标回收率为72.8%~110.8%,相对标准偏差RSD为5.5%~16%。与传统方法相比,该法无需对有机污染物进行分类处理,可以同时快速测定7类27种有机农药。     

《化学通报》网络版（Chemistry Online）2004年第3期论文摘要

[w0 17]多金属氧酸盐光催化降解水中有机污染物Photocatalytic Degradation of Organic Pollutantsin Waterby Polyoxometalates朱秀华　朱　敏　王　炜 (大连铁道学院环境科学与工程系　大连　 116 0 2 8)介绍了多酸的一般性质 ,对多金属氧酸盐在均相和多相水环境中光催化降解有机污染物的催化性能和机理进行了综述。重点介绍了多余属氧酸盐及固载多金属氧酸盐对水中有机氯化物、农药及染料的光催化性能并与 Ti O2 、H2 0 2 的光催化活性和机理进行了比较。The basic characters of polyacid and research progress on photocatalytic …     

固相萃取-液相色谱-离子阱二级质谱法同时测定饮用水中多种痕量有机污染物

建立了高效液相色谱-离子阱二级质谱法同时测定饮用水中内分泌干扰物、农药残留和丙烯酰胺等15种痕量有机污染物的方法。250mL水样先用C18固相萃取柱富集,经梯度洗脱液相色谱分离,采用时间分段的方法确定各组分质谱检测条件,利用离子阱二级质谱进行测定。所检测的15种有机污染物定量线性关系良好,相关系数为0.9975～0.9998,检测限在0.2～20ng/L之间。在低、中、高3个不同加标水平下,实际水样的加标回收率为75.1%～99.5%,相对标准偏差为4.6%～12.3%。该方法成功用于5种不同来源饮用水样的检测,获得了满意结果。     

水中烷基汞的检测方法研究进展

烷基汞是一类毒性较大的有机污染物,近年来多次引发污染事件,引起人们的广泛关注。对水中烷基汞的检测标准和测定方法的研究进展进行了综述,并对各种检测方法的优缺点进行了比较。     

金属纳米团簇在农药检测中的应用研究进展

农药对提高农作物质量和产量具有重要作用,然而,过量以及不合理使用农药导致的残留和污染对人类健康及环境均具有严重危害,因此对农药及其残留的检测尤为重要。金属纳米团簇（Metal nanoclusters,MNCs）作为一种新型纳米材料,具有尺寸小、稳定性高、易制备和生物相容性好等优点,在分析传感领域备受关注。MNCs在农药检测方面也展现出巨大的应用潜力。本文综述了近年来基于MNCs的检测方法以及在有机磷农药、有机氮农药和有机氯农药等常见农药检测中的研究进展,并对其在农药检测方面的发展前景进行了展望。     

基于环糊精的农药吸附剂的研究进展

农药的研发与使用极大地提高了农作物的产量,为解决人类温饱、改善人类生活品质做出了贡献。但是,农药广泛残留于农副产品以及土壤和水体中,造成的污染日趋严重。残留的农药通常具有微量致毒、难生物降解、生物累积等特性,对生物健康与生态系统造成了巨大威胁。高效检测微量农药、减小污染危害是亟待解决的问题。吸附法具有成本低、操作简单、稳定性强、可重复性强的特点,在农药分离预富集领域得到了广泛关注。作为一种常用的农药吸附剂材料,环糊精是一类具有空腔的超分子化合物,能够作为主体通过主客体作用形成包合物;另外,可以通过醚化、酯化、氧化等化学反应对环糊精进行后修饰以提高其吸附性能。疏水作用、静电作用、范德华力、氢键作用、立体效应协同促进对农药的吸附。环糊精在农药吸附领域已经取得了一定进展,但是目前还没有基于环糊精的农药吸附剂的综述。该文针对杀菌剂、杀虫剂、除草剂、植物生长调节剂这4类农药,系统性地评述了基于环糊精的农药吸附剂的制备、吸附机理及应用,目前存在个别吸附剂吸附容量不高、降解机理不明确、降解产物对环境不友好、容易造成二次污染的问题,研发高吸附容量、易回收、易分离、易再生的基于环糊精的农药吸附剂是未来的主要研究方向。     

碳素基体固相微萃取吸附质的研制

研制了石墨型碳素基体固相微萃取吸附质,并以该新型固相微萃取装置联用气相色谱 电子捕获检测器分析水体中的有机农药。考察了吸附萃取时间及离子强度对分析结果的影响,并与商品装置进行了对比,结果表明其具有很好的应用前景。     

Application of Compound-Specific Isotope Analysis in Environmental Forensic and Strategic Management Avenue for Pesticide Residues

Unintended pesticide pollution in soil, crops, and adjacent environments has caused several issues for both pesticide users and consumers. For users, pesticides utilized should provide higher yield and lower persistence while considering both the environment and agricultural products. Most people are concerned that agricultural products expose humans to pesticides accumulating in vegetation. Thus, many countries have guidelines for assessing and managing pesticide pollution, for farming in diverse environments, as all life forms in soil are untargeted to these pesticides. The stable isotope approach has been a useful technique to find the source of organic matter in studies relating to aquatic ecology and environmental sciences since the 1980s. In this study, we discuss commonly used analytical methods using liquid and gas chromatography coupled with isotopic ratio mass spectrometry, as well as the advanced compound-specific isotope analysis (CSIA). CSIA applications are discussed for tracing organic pollutants and understanding chemical reactions (mechanisms) in natural environments. It shows great applicability for the issues on unintended pesticide pollution in several environments with the progress history of isotope application in agricultural and environmental studies. We also suggest future study directions based on the forensic applications of stable isotope analysis to trace pesticides in the environment and crops.     

Development of methods for determination of the residues of 15 pesticides in medicinal herbs Isatis indigotica Fort. by capillary gas chromatography with electron capture or flame photometric detection

Two multiresidue methods were developed for the determination of 15 pesticides (organochlorines, organphosphorus compounds, pyrethroids, and fungicides) in medicinal herbs Isatis indigotica Fort. and its formulations. The analytical procedure is based on ultrasonic assisted extraction and liquid-liquid extraction (LLE). After solvents were added, the raw material or granule sample was sonicated in an ultrasonic water bath and then centrifuged, filtered, and cleaned up by LLE. The infusion sample was extracted with petroleum ether by LLE. The pesticide residues were determined by capillary gas chromatography with electron-capture or flame photometric detection. Recoveries with the method at concentrations between 0.4 microg/kg and 10 mg/kg ranged from 70.2 to 119.5% for raw material, 73.2 to 105.1% for granule formulation, and 72.8 to 113.3% for infusion formulation. The relative standard deviation values were <20% for all of the pesticides studied. The pesticide detection limits were within the ranges 0.3-0.5 microg/L for endosulfan, 3-7.5 microg/L for pyrethroids, 0.7-32.5 microg/L for organophosphorus pesticides, and 0.1-0.6 microg/L for the other pesticides. The proposed methods are simple and rapid and provide simultaneous determination of pesticide residues in Isatis indigotica Fort. with acceptable recoveries and repeatability and an adequate limit of determination.     

Determination of 24 pesticides residues in mineral and peat soils by modified QuEChERS method and gas chromatography

A simple extraction and cleanup procedure has been developed for the analysis of 24 organophosphorus (OP), organochlorine (OC) and pyrethroid (PY) pesticides in mineral and peat soils using modified QuEChERS method. The pesticides were extracted from the soil with acidified acetonitrile. The water was removed from the extract by salting out with sodium chloride and addition of magnesium sulfate. For OP pesticides, the extracts were cleaned up with 0.2 g of primary secondary amine packed in glass Pasteur pipette and determined by gas chromatography with flame photometric detector. For OC and PY pesticides, the extracts were cleaned up with 0.2 g of silica gel packed in a glass Pasteur pipette and determined by gas chromatography with electron capture detector. After the cleanup, the extracts had lower colour intensity and reduced matrix interferences. The recovery of the OP and OC pesticides for mineral and peat soils determined at 0.01–1.0 mg kg^?1 fortification levels ranged from 79.0–120.0% and 82.2–117.6%, respectively. The detection limits for OP and OC pesticides were 0.001–0.01 and 0.002–0.005 mg kg^?1, respectively. The recovery of the PY pesticides ranged from 87.5–111.7% at the detection limits of 0.002–0.010 mg kg^?1. The relative standard deviations for all pesticides studied were below 10.8%. The modified method was simple, fast, and had utilized less reagents than the conventional methods. The method was applied to the determination of the pesticide residues in mineral and peat soil samples collected from the vegetable farms.     

Applications of solid‐phase micro‐extraction with mass spectrometry in pesticide analysis

Pesticides, widely applied in agriculture, can produce a variety of transformation products and their continuous use causes deleterious effects to ecosystem. Efficient and sensitive analytical techniques for enrichment and analysis of pesticides samples are highly required. Compared with other extraction methods, solid‐phase micro extraction is a solvent free, cost effective, robust, versatile, and high throughput sample preparation technique, especially for the analysis of pesticides from complicated matrices. Coupling of solid‐phase micro extraction with gas chromatography and mass spectrometry and liquid chromatography–mass spectrometry has been extensively applied in pesticide analysis. On the other hand, in recent years, combination of fast separation using solid‐phase micro extraction and rapid detection using ambient mass spectrometry is providing highly efficient pesticide screening. This article summarizes the applications of solid‐phase micro extraction coupled to mass spectrometry for pesticides analysis.     

高分辨质谱技术在农药残留检测中的应用

农药残留检测是农产品中有害物质控制的重要组成部分,随着农药残留限量标准体系的发展完善,农药残留检测方法也在不断进步。近年来质谱技术发展迅速,已被广泛应用于农药残留检测领域,高分辨质谱由于具有较高的分辨率和质量精确度,在复杂基质的农药多残留高通量检测中发挥着越来越重要的作用。本文从高分辨质谱与液相色谱、气相色谱及其他分离模式联用等方面出发,简述了近5年来高分辨质谱在农药残留检测中的应用,对目前高分辨质谱在农药残留检测应用中发现的问题进行了讨论,并对其未来发展趋势进行展望。     

A review of sampling approaches to off-target pesticide deposition

Off-target deposition is one of the major routes of pesticide entry into the environment. Several studies have been carried out employing different tracers in an attempt to estimate pesticide deposition in the environment. This paper, in contrast, reviews different off-target sampling methods using the pesticide active ingredient. A critical analysis has been conducted on the sampling methods as applied to (a) pesticides of different volatilities, (b) samplers constructed using different materials, and (c) global distribution of the studies carried out on different pesticides using these samplers. In the last twenty years, pesticide deposition sampling has been carried out using various samplers such as chromatography paper, glass and plastic petri dishes, glass microscope slides, stainless steel rods and discs, amongst others. Of these, most studies have reported the use of chromatography paper because of the numerous advantages that it possesses, including protecting the pesticides from photodegradation and volatilisation. Air dispersion software models applied to pesticide deposition have tended to either over-predict or under-predict the amount of surface deposition resulting from pesticide spray drift. In conclusion, more work needs to be done to standardise pesticide deposition monitoring methods, including the choice of the most appropriate sampler for a particular situation, in order to obtain comparable and accurate data.     

A novel chemiluminescence assay of organophosphorous pesticide quinalphos residue in vegetable with luminol detection

Background  

Organophosphorous pesticides are the most popular pesticides used in agriculture. As acetylcholinesterase inhibitors, organophosphorous pesticides are toxic organic chemicals. The control and detection of organophosphorous pesticide residue in food, water, and environment therefore plays a very important role in maintaining physical health. A sensitive, rapid, simple chemiluminescence(CL) method has been developed for the determination of quinalphos based on the reaction of quinalphos with luminol-H₂O₂ in an alkaline medium. The method has been applied to detection of quinalphos in vegetable samples with satisfactory results.