我国水环境有机物分析前处理技术

介绍了我国水环境有机物分析中常用的前处理技术,包括液液萃取、树脂吸附、固相萃取、固相微萃取、液膜萃取、半透膜被动采样、顶空、吹扫-捕集等,归纳了各种方法的原理、应用及优缺点,并对环境中有机污染物前处理技术的发展方向进行了展望。     

无锡市水源地致嗅物质调查及原因分析

运用吹扫捕集及固相微萃取前处理方法,采用气相色谱-质谱法建立无锡水源地中致嗅物质谱库,调查分析了2009年无锡市饮用水水源地水体中致嗅物质的组成和浓度水平,并对饮用水源地水中致嗅物质进行成因分析.     

我国环境中有机污染物分析方法及痕量富集技术的进展

综述了我国环境中有机污染物的分析方法和痕量富集技术，介绍了吹扫-捕集法、固相微萃取技术、固相萃取技术、半渗透膜采样技术与分析仪器联用在有机污染物测定中的应用情况。     

太湖水源水主要异味物质变化规律及来源初探

采用顶空固相微萃取-气相色谱/质谱联用测定技术,以太湖某饮用水源地水体中甲基异莰醇-2和土臭素为主要研究对象,通过环境因子相关性分析,对异味物质的变化规律和来源作初步分析。研究结果表明,该水源地2013年的主要异味物质为甲基异莰醇-2,超标时段主要集中在夏秋高温季节(5—9月);水体中的硅藻可能是异味物质的重要产生者,底泥中的藻类和微生物次生代谢活动可能是水体产生异味的主要原因。     

固相微萃取技术在环境监测分析中的应用进展

样品前处理是整个样品分析过程中的关键一环,其目的在于减少杂质对待测物的干扰及对目标物进行富集。固相微萃取技术是集采样、萃取、富集、进样于一体的样品前处理新技术。近年来,固相微萃取技术在环境污染物监测分析领域得到了广泛应用,该文章系统地综述了固相微萃取技术在不同环境基质(水体、大气、土壤及沉积物)预处理的方法,比较了不同类型涂层材料(如纳米材料、离子液体等)与装置形式(如内部冷却固相微萃取、箭形固相微萃取等)的优缺点及应用范围。针对现阶段固相微萃取技术应用于不同环境基质中存在的问题和不足,提出进一步研究的方向。     

藻型湖泊大量藻类衰亡后致嗅物的分析以及水质变化的研究

藻类大量死亡后极易产生致嗅物.我们模拟了藻类的生长死亡过程,观测除藻后水体理化性质和生物性质的改变情况以及致嗅物的成分及浓度,以确定致嗅物质产生的途径.由于藻类死亡后细胞解体,藻类细胞中的氮、磷物质释放到水体中,导致水体的富营养化程度反而升高,而叶绿素-a也呈现下降趋势,整个试验过程后期溶解氧为0,水体产生嗅味物质,可采用吹扫捕集/固相微萃取—气相色谱—质谱法和顶空固相微萃取气质联用法分析致嗅物质.实验证明,当藻型湖泊的藻类被基本去除后,整个水体的初级生产力受到严重的破坏,威胁到水生态系统的安全性,可导致水体进一步恶化.     

固相微萃取-气相色谱在水中有机污染物测定中的应用

固相微萃取技术是一种新型的无溶剂的样品前处理方法,集取样、萃取、富集、进样于一体,具有无溶剂、可直接进样、操作简便快捷、灵敏的特点。简述了固相微萃取技术原理,综述了SPME与GC联用在水中有机污染物测定中的应用。具体介绍了该技术在苯系物、酚类化合物、多环芳烃、有机氯化物及其它有机污染物分析中的应用,并提出了该技术的发展趋势及应用展望。     

磁性分散固相萃取气相色谱法测定地表水中有机磷化合物

应用磁性分散固相萃取技术对环境水体中有机磷化合物进行萃取测定,并对萃取剂的用量、萃取时间、解吸溶剂、盐度等实验影响因素进行了优化。在优化条件下,有机磷的回收率为80.1%~93.1%,相对标准偏差为4.6%~5.9%,检出限为0.000 2~0.000 4 mg/L。与传统的液液萃取及固相萃取相比,该磁性分散固相萃取方法操作更为简单、迅速,有机溶剂消耗量很少,方法环保。能很好的满足环境水体中有机磷化合物的测定。     

不同环境介质中抗生素的污染现状及其检测方法研究进展

综述了环境中抗生素的来源、国内外不同环境介质中抗生素的污染水平及检测方法。现有研究表明,抗生素污染已遍布土壤、水体、动植物组织等介质中,且国内抗生素污染水平较国外相对偏高。通过不同检测技术的优劣对比,得出固相萃取技术与液相色谱质谱联用技术是目前最常用的样品前处理技术和检测方法,具有灵敏度高和精确度好的特点。     

水中有机磷农药分析前处理方法探讨

分别采用液-液萃取、固相萃取前处理方法,提取水中10种常见的有机磷农药,对比了这两种提取方法的测定结果、经济成本、花费时间及对环境的影响,建议逐步用固相萃取法取代液？液萃取法提取水中有机磷农药。     

水中微囊藻毒素的超高效液相色谱-串联质谱法研究

建立测定水体中微囊藻毒素(MCYST)的超高效液相色谱-串联质谱分析方法.水样通过固相萃取富集净化,采用超高效液相色谱-串联质谱测定,6min内完成3种MCYST的分离及检测.MCYST-LR、MCYST-RR、MCYST-YR检出限分别为3.5、2.5、5.0ng/L,回收率为85.6％～107.9％,为水质微囊藻毒素监测提供了一种快速、准确、灵敏的分析方法.     

固相萃取-超高效液相色谱-串联质谱法同时测定地表水中9种性激素

建立了地表水中9种性激素的固相萃取-超高效液相色谱-串联质谱检测方法。利用HLB固相萃取柱富集水体中痕量性激素,用甲醇洗脱并浓缩,再以1 mmol/L氟化铵-乙腈为流动相,经C_(18)柱分离,采用电喷雾离子源、质谱多反应监测模式,内标法定量,实现了地表水中9种性激素的同时检测。方法检出限为0. 1～1. 8 ng/L,在低、中、高3个加标水平下,性激素的平均回收率为69. 6%～115. 0%,相对标准偏差为3. 2%～17. 7%。该方法灵敏度高,定性准确,操作简单高效,适用于地表水中9种性激素的定性定量分析。     

长江南京段新兴污染物污染特征及风险评估

在长江南京段上游至下游依次布设6个采样点采集水样,使用固相萃取和LC-MS/MS相结合的方法对5种选定药物的质量浓度进行测定,并采用风险熵模型评估其生态风险。结果表明,6个采样点均检测到药物存在。其中,四环素、红霉素、罗红霉素和氯霉素的检出率为100%,最高检出值为10.29 ng/L(氯霉素)。与国内外其他地表水相比,长江南京段水中的药物质量浓度较低。生态风险评估结果表明,长江南京段水中5种药物的风险熵值均低于1,对水生生物不存在高风险。     

超高效液相色谱三重四级杆质谱联用法测定水中的氯霉素

建立了固相萃取一超高效液相色谱三重四级杆质谱联用法同时测定水中痕量的氯霉素残留，该方法采用电喷雾电离源、多重反应监测负离子模式在5min内完成对氯霉素的分析，方法检出限为0．2ng/L，空白样品和实际样品的加标回收率为76．2％～104％，该方法具有操作简便，灵敏度高，重现性好的特点。     

Preliminary studies of a fast screening method for polycyclic aromatic hydrocarbons in soil by using solvent microextraction-gas chromatography

Solvent microextraction (SME) was applied to the extraction of polycyclic aromatic hydrocarbons (PAHs) from spiked and real environmental soil samples with different matrices. Soil sample was mixed with 7 mL of acetone and 14 mL of water to allow partitioning of the PAHs from the soil to the liquid phase. A 2 microL octane drop suspended from a microsyringe needle tip was then immersed into the stirred solution-soil mixture for extraction. After an 11 min extraction, the octane drop was withdrawn into the syringe and injected directly into the GC for identification and quantification. The whole analysis procedure took 27 min, with an extraction time of 11 min, and a GC separation time of 16 min. A second extraction could be undertaken whilst the GC is running, hence the GC run time currently limits the sample throughput. In this method, a small amount of organic solvent was used for the extraction process, which produced little waste. The limits of detection for lower molecular weight (< 230) PAHs range from 0.13 to 0.36 mg kg-1, and for higher molecular weight (> 250) PAHs are estimated to be between 0.5 and 1.0 mg kg-1, with RSD values generally under 20%. Due to the small volumes of organic solvent used, the consumable cost per extraction is only US$ 0.12. This is the first report of the application of SME to solid samples, and the first report of the use of SME for the analysis of PAHs.     

固相萃取-超高效液相色谱-串联质谱法快速测定环境水样中30种极性农药

建立了固相萃取-超高效液相色谱-串联质谱快速测定环境水样中30种极性农药的方法。30种极性农药经过固相萃取(SPE)富集净化,以超高效液相色谱-串联质谱(UPLC-MS-MS)多级监测模式(MRM)外标法进行定性定量分析。结果表明:环境水样中30种极性农药的检出限为0.2～5 ng/L。对同一环境样品进行了低、中、高3个不同浓度水平的加标回收实验,平均回收率为63.7%～105.1%,相对标准偏差为4.4%～21.2%。该方法快速、灵敏、准确,可有效应用于环境水样中30种极性农药的快速监测。     

Injectors for capillary gas chromatography and their application to environmental analysis

The application of different injectors in capillary gas chromatography (GC) analysis of semi-volatile organic contaminants in environmental samples prepared in organic solvents is reviewed. The injectors examined include a split/splitless injector in splitless mode (SS), cold on-column (COC), and programmable temperature vaporizer (PTV) and adaptations of these injector designs. Key issues when selecting an injector include properties of the analyte, such as potential for thermal degradation or discrimination of high boiling point compounds within the injector, and the ability of the GC systems to handle large volume injections (LVI) primarily to lower detection limits and allow direct coupling with sample preparation techniques such as at-line or on-line solid phase extraction (SPE). LVI also require consideration of matrix interference issues. This review examines only injector chamber modifications that are feasible with a standard GC configuration, however some modifications to the chromatographic system to extend the range of applicability of gas chromatography analysis for environmental samples are also noted.     

水体中磺胺、四环素、喹诺酮类抗生素检测方法

建立了固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)同时检测水体中3类15种抗生素的分析方法。水样用Oasis HLB固相萃取小柱净化富集。通过对比水样在不同pH条件下的回收率,优化了环境水样中抗生素固相萃取过程中的前处理条件。采用甲醇和0.1%甲酸溶液作为流动相,经过梯度洗脱进行分离,在HPLC-MS/MS多反应监测模式下进行定性定量分析。结果表明,环境水体中15种抗生素的检出限和定量下限分别为0.12~1.6 ng/L和0.2~3.0 ng/L,自来水加标回收率为34.9%~102.5%(pH=4)。用该方法对海河流域13个地表水水样进行了初步检测,结果表明,部分抗生素普遍存在于地表水体中。其中,磺胺甲基异NFDA1唑检出频率最高,在13个地表水样品中均有检出。     

Simultaneous analysis of endosulfan, chlorpyrifos, and their metabolites in natural soil and water samples using gas chromatography-tandem mass spectrometry

Analysis of endosulfan, chlorpyrifos, and their nonpolar metabolites in extracts from environmental aqueous and soil samples was performed using a gas chromatography-tandem mass spectrometry (GC–MS/MS) technique. Full-scan GC–MS analysis showed poor sensitivity for some of the metabolites (endodiol and endosulfan ether). A multisegment MS/MS method was developed and MS/MS parameter isolation time, excitation time, excitation voltage, and maximum excitation energy were optimized for chosen precursor ions to enhance selectivity and sensitivity of the analysis. The use of MS/MS with optimized parameters quantified analytes with significantly higher accuracy, and detection limits were lowered to ~1/6th compared with the full-scan method. Co-eluting compounds, chlorpyrifos and chlorpyrifos oxon, were also analyzed successfully in the MS/MS mode by choosing exclusive precursor ions. Analysis of soil and water phase samples from contaminated soil slurry bioreactors showed that the MS/MS method could provide more reliable estimates of these pesticide and metabolites (especially those present in low concentrations) by annulling interferences from soil organic matter.