GC-MS检测济南市东部空气中气相与颗粒物上有机污染物

用GDX-101吸附剂和玻璃纤维滤膜(GF)同时采集气相和颗粒物上有机污染物,样品经提取分离后用GC-MS进行定性分析.结果表明,颗粒物上有机污染物的种类和含量都高于气相,工业区空气中有机污染较生活区严重,仍以燃煤、燃油污染为主.     

预冷冻浓缩系统与气相色谱-质谱联用测定空气中挥发性有机物

采用预冷冻浓缩系统和气相色谱-质谱联用,建立了测定空气中39种挥发性有机物的分析方法,该法用苏玛罐或Tedlar气袋采集空气样品经-160℃液氮预冷冻浓缩后,用GC-MS检测.该方法采样简便,灵敏度、准确度高,已应用于室内空气和环境空气的测定,取得满意的结果.     

Profiling the spatial concentration of allethrin and piperonyl butoxide using passive sorptive sampling and thermal desorption capillary GC-MS

Spatial concentration distribution of a chemical in an indoor environment is an important factor in the evaluation of chemical nuisances. However, straightforward techniques for the determination of this distribution are not very common and usually limited in their application. Sorptive sampling using polydimethylsiloxane-coated stir bars and the combination of active and diffusive sampling were shown to allow uncomplicated spatial concentration profiling of multiple compounds in an indoor environment. The validity of the approach was demonstrated in the analysis of the spatial concentration distribution of a pyrethroid insecticide in a common bedroom. The relative concentrations of allethrin and piperonyl butoxide were profiled throughout the room upon the application of an insecticide vaporizer.     

Octyl and nonylphenol ethoxylates and carboxylates in wastewater and sediments by liquid chromatography/tandem mass spectrometry

This work presents an LC–MS–MS-based method for the quantitation of nonylphenol ethoxylates (NPEOs) and octylphenol ethoxylates (OPEOs) in water, sediment, and suspended particulate matter, and three of their carboxylated derivatives in water. The alkylphenol ethoxylates (APEOs) were analyzed using isotope dilution mass spectrometry with [¹³C₆]-labeled analogues, whereas the carboxylated derivatives were determined by external standard quantitation followed by confirmation using standard additions. The method was used to study APEO’s behavior in a wastewater treatment plant (WWTP), where total dissolved NP0-16EO concentration was reduced by approximately 99% from influent (390 μg l⁻¹) to final effluent (4 μg l⁻¹), and total OP0-5EO concentration decreased by 94% from 3.1 to 0.2 μg l⁻¹. In contrast, the carboxylated derivatives were formed during the process with NP0-1EC concentrations increasing from 1.4 to 24 μg l⁻¹. Short-chain APEOs were present in higher proportions in particulate matter, presumably due to greater affinity for solids compared to the long-chain homologues. NP (0.49 μg l⁻¹) and NP0-1EC (4.8 μg l⁻¹) were the only APEO-related compounds detected in a surface water sample from a WWTP-impacted estuary; implying that 90% of the mass was in the form of carboxylated derivatives. Sediment analysis showed nonylphenol to be the single most abundant compound in sediments from the Baltimore Harbor area, where differences in homologue distribution suggested the presence of treated effluent in some of the sites and non-treated sources in the rest.     

Characterization of humic substances of different origin by means of mass spectrometry and neural networks

Mass spectrometry fingerprinting of humic acids extracted from different soils has been carried out using laser desorption/ionization mass spectrometry (LDI-TOF MS). LDI-TOF MS provides characteristic mass spectra fingerprints for the humic acids of different origin. The information given in the fingerprints was evaluated for natural grouping trends in the samples by neural networks computing tools, such as self-organizing feature map (SOFM). This approach is efficient for recognizing patterns in the humic acids samples independently of their characteristic variability; variability characterizing natural products such as humic substances. The use of multi-layer perceptron artificial neural networks gave a successful classification of the samples.     

气-水界面对病毒静态吸附实验结果的影响

气-水界面存在可能导致不能正确评价土壤对病毒的静态吸附能力.本研究通过室内一次平衡法实验,比较分析气-水界面对噬菌体MS2在不同处理（非灭菌/灭菌）的不同土壤中的吸附实验结果影响,同时评价不同程度气-水界面对没有土壤存在时的病毒回收率影响.结果表明,气-水界面存在对吸附实验结果的影响在砂质潮土上最为明显,其次为红壤土,而在红粘土上的影响几乎可忽略,这可能与土壤本身吸附/致死病毒的能力不同有关;土壤灭菌后进一步加剧气-水界面对砂质潮土吸附实验结果的偏差,而在红壤土上则有减弱趋势.气-水界面存在显著降低空白实验病毒回收率,其降低趋势随气-水界面的增加而加剧,当加入土壤后,土壤颗粒有可能阻止病毒接近气-水界面或改变病毒吸附在固-液-气界面的力量,因而气-水界面存在时的空白实验结果并非为真正的空白实验结果,这可能是导致气-水界面引起静态吸附实验结果偏差的主要原因.     

水中微量弱极性内分泌干扰物测定方法的研究

使用ENVITM Chrom P固相萃取小柱、双(三甲基硅烷基)三氟乙酰胺(BSTFA)衍生剂及气质联机,系统研究了水中弱极性内分泌干扰物(EDCs)的测定方法.通过正交试验,得到最佳固相萃取条件为:水样流速5 mL/min,洗脱剂为二氯甲烷,洗脱速率0.5 mL/min,洗脱剂体积6 mL.最佳衍生化条件为:BSTFA 100 μL,60 ℃,反应时间30 min.结果表明,双酚A、五氯酚、2,4-二氯苯酚、4-壬基酚、雌二醇、雌三醇、雌酮、炔雌二醇的回收率在82.4%～101.9%,检出限为0.01～0.06 μg/L.     

SPE-HPLC/MS联用法测定地表水中的PFOA及PFOS含量

本文建立了固相萃取与高效液相色谱／质谱（HPLC／MS）联用的方法来测定地表水中全氟辛酸（PFOA）及全氟辛烷基磺酸（PFOS）的含量。此方法中PFOA在水样中的线性范围为40ng／L到500ng/L，线性相关系数0．9986，PFOS在水样中的线性范围为5n异／L到500ng/L，线性相关系数0．9905。此方法中全氟辛酸及全氟辛烷基磺酸的平均回收率分另13为83.91％和86.63％。水样中全氟辛酸和全氟辛炕基磺酸的检出限均为0.5ng／L。方法准确、可靠，分析结果令人满意。采用此方法测定了上海部分地区地表水中全氟辛酸及全氟辛烷基磺酸的含量。实验结果表明，上海地区长江入海口处徐六泾段全氟辛酸的平均浓度是46．88ng／L，全氟辛烷基磺酸未检出；黄浦江段全氟辛酸及全氟辛烷基磺酸的平均浓度分别是1594．83ng／L（前处理后需稀释10倍以确保在方法线性范围内）和20．46ng/L。可见长江及黄浦江流域的全氟辛酸及全氟辛烷基磺酸的控制与治理亟待提上议程。     

Improved liquid chromatographic photo diode array mass spectrometric determination of 5-hydroxymethylfurfural and related furfurals in honey

5-Hydroxymethylfurfural is found in several food commodities, including honey. Its concentration is used as one of honey's quality indicators since elevated 5-hydroxymethylfurfural levels indicate overheating and aging of the product. In this context, the European Commission and Codex Alimentarius established the maximum tolerable level for 5-hydroxymethylfurfural, for general type honeys intended for human consumption, at 40 mg kg^?1. In this study, 5-hydroxymethylfurfural, 2-furfural, and the furfuralic derivative 5-methyl-2-furfural were investigated in Greek honey samples, through a high performance liquid chromatographic photo diode array mass spectrometric method developed and validated. Sample preparation was based on a modification of the ‘Quick, Easy, Cheap, Effective, Rugged, and Safe’ procedure. The method was sensitive, exhibiting limit of detection for 5-hydroxymethylfurfural at 0.1 mg kg^?1, far below the permissible level of 40 mg kg^?1. Levels of 5-hydroxymethylfurfural in 28 honey samples varied from 0.5 to 23.5 mg kg^?1, thus, not worrying for consumers. Traces of 2-furfural were detected in limited samples.     

自来水处理工艺对溶解相中全氟化合物残留的影响

为探究自来水原水到出厂水各处理环节对自来水中全氟化合物(perfluorinated compounds,PFCs)残留的影响,了解原水中PFCs的季节性变化规律,应用WAX固相萃取分离富集与高效液相色谱-质谱联用相结合的方法,分析了深圳市某自来水厂一年间原水、出厂水及絮凝池、沉降池、砂滤池、臭氧+活性炭池出水溶解相中13种PFCs的残留水平.结果表明,原水和出厂水中ΣPFCs残留呈春夏高而秋冬低的趋势,检出的PFCs呈中短链(C≤10)长链(C≥11)的分布,而全氟辛烷磺酸是PFCs最典型残留种态.在原水经过的5个处理环节中,臭氧+活性炭、沉降和砂滤具有PFCs去除效应,然而絮凝和液氯消毒却分别使短链(C≤6)和中链(10≥C≥7)PFCs显著上升,导致出厂水中ΣPFCs浓度较原水增加了10%～44%.但出厂水中PFCs残留远低于其限值,尚不足以影响人体健康.