基于GC-QTOF/MS的大气中有机污染物的非靶标筛查及半定量分析

本文借助气相色谱-四极杆飞行时间质谱仪(GC-QTOF/MS)开展了大气中有机污染物的非靶标筛查,并对识别出的特征污染物进行半定量分析.基于高分辨质谱数据库和NIST质谱数据库的匹配,样品中共识别出139种污染物,主要以多环芳烃(PAHs)及其衍生物、邻苯二甲酸酯(PAEs)为主;除此之外,还识别出多种尚未受到监管的杂...     

气相色谱-四极杆-飞行时间质谱仪(GC-QTOF)分析土壤中多环芳烃和农药残留

采用气相色谱-四极杆-飞行时间质谱(GC-QTOF)结合振荡提取方式对土壤中农药和多环芳烃进行准确鉴定.利用TOF精确质量数的提取可以有效的抗干扰,得到准确的结果.对土壤样品在0.1 mg·L-1浓度水平进行添加回收率测定,大部分农药和多环芳烃的回收率结果在70.0%—120.0%之间,相对标准偏差小于15.0%.在0.01 mg·L-1浓度水平下大部分的农药和多环芳烃在土壤基质中均能被检测出来,有很好的灵敏度.本方法操作简单、快速、灵敏度高,能够对土壤中痕量多组分农药残留和多环芳烃进行准确的定性和定量分析.     

气相色谱串联三重四极杆质谱在持久性有机污染物分析中的应用

三重四极杆质谱的多重反应监测模式适合痕量有机化合物的分析,应用气相色谱串联三重四极杆质谱(GC-MS/MS)检测多环境介质中持久性有机污染物有逐年增多的趋势.本文综合评述了GC-MS/MS在水体、大气、土壤、沉积物和生物样品中持久性有机污染物分析方面的应用.     

气相色谱-四极杆-飞行时间质谱仪（GC-QTOF）分析大葱中多种农药残留

大葱不仅是中国传统的调味品,而且是一种重要的出口农产品.传统的分析方法,比如气相色谱或者气相色谱-单四极杆质谱仪容易受大葱当中强基质干扰,造成分析结果出现偏差.     

气相色谱-质谱联用内标法测定土壤中11种酞酸酯

建立了土壤中11种酞酸酯(PAEs)的气相色谱-质谱联用(GC-MS)内标分析方法,通过优化色谱柱升温程序和载气流量后,11种酞酸酯在18 min内得到良好的分离.同时以连续7次进样后计算PAEs峰面积响应值和峰面积变异系数为衡量指标,并逐个优化GC-MS的进样口温度、GC与MS的接口温度、进样方式和进样体积等GC-MS仪器操作参数,确定了GC-MS分析PAEs的最优条件为进样口温度250℃,接口温度280℃,载气流速1.2 mL.min-1,进样体积1.0μL,非脉冲进样方式.该分析条件下PAEs各组分的检出限(S/N=3)为0.37—1.97μg.L-1.该分析方法用于土壤样品中酞酸酯含量分析,并用苯甲酸苄酯(BenzylBenzoate)作为内标物,用内标法对11种肽酸酯进行定量,方法检出限0.01—0.07 mg.kg-1,土壤加标回收率基本在93.0%—115.0%范围内,结果可行.     

土壤柱气相色谱法研究土壤中有机污染物的热脱附行为

采用土壤柱气相色谱法研究了四种有机污染物在土壤上的热脱附动力学特征,以及容量因子(k')同有机污染物的主要理化参数的数学关联.结果表明,有机污染物在土壤上的慢脱附过程符合双常数方程;并且随温度的升高,lg k'和拖尾因子(Tf)均呈直线降低.lg k'与lg Kow,lg Koa和lg Koc以及沸点(TB)均呈极显著的直线相关,其中,lg k'与lg Koa和TB的相关系数值很高,分别为0.978和0.966,说明二者可以很精确的预测有机污染物在土壤中的热脱附速率.     

沥青烟化学组分的气相色谱-质谱联机分析

沥青烟是一种特殊的污染物,沥青烟由液态烃类颗粒物和气态烃类衍生物组成,所含多环芳烃（苯并（a）芘）对人体危害很大,它主要来自碳素行业焙烧炉和浸渍工序,炼铝业焙烧炉,道路沥青石子生产和化工行业沥青制品工序和防水材料建筑业涂浸等。为治理和控制沥青烟的污染,辽宁省环境保护局于1989年制定了沥青烟排放标准,并注明沥青烟以苯溶物为执行标准。1996年国家制定新的大气污染物综合排放标准,增设了沥青烟和苯并（a）芘排放标准,根据监测分析工作的需要,我们研制了沥青烟富集器,用涂有色谱固定液的玻璃纤维滤筒捕集沥青烟和多环芳烃,用烟尘测试仪进行等束采样,同时采集沥青烟尘和捕集气态烃类物质。我们对沥青烟样品进行了气相色谱－质谱联机分析,共检出了196种有机污染物,主要化学组分是多环芳烃。     

气相色谱／质谱测定电子垃圾拆解区土壤中四溴双酚A的方法

本研究建立气相色谱/质谱来测定电子垃圾拆解区土壤中四溴双酚 A（TBBPA）的方法。该化合物通过超声波辅助萃取,溶剂选择V（丙酮）﹕V（正己烷）=1﹕1或乙酸乙酯;净化柱选择酸化的氟罗里硅土和无水硫酸钠混合物或CleanertC18-SPE进行净化;净化液浓缩后经衍生反应,衍生试剂选用N,O-双（三甲基硅烷基）三氟乙酰胺（BSTFA）和含1%的三甲基氯硅烷（TMCS）。该方法测定电子垃圾拆解区土壤中TBBPA的检出限为（S/N=3）0.1μg·kg^-1加标回收率平均值为92.7%（n=5）,重现性RSD为2.52%（n=5）;线性范围是20～400μg·kg^-1相关系数0.999。该方法用于调查电子垃圾拆解区土壤中四溴双酚A,范围值为5.17～218.00μg·kg^-1其周围农田土壤中四溴双酚A,范围值为0.312～4.170μg·kg^-1     

Nuclear magnetic resonance studies of interactions between organic pollutants and soil components,a review

This article presents a short overview of selected recent papers using nuclear magnetic resonance (NMR) to investigate interactions between organic pollutants and soil components such as organic matter, clays, whole soils, and sediments. First, we describe solid state cross polarisation magic angle spinning (CP-MAS) experiments as the main tools to investigate covalent bonds. Second, we report NMR approaches allowing us to assess molecule mobility and to characterise non-covalent interactions. Those approaches include correlations between K _oc values and soil organic matter functions determined by CP-MAS, ²H NMR fingerprints, relaxation time measurements, ¹⁹F and ¹H high resolution (HR)-MAS experiments.     

石墨烯在环境有机污染物分析中的应用进展

石墨烯是一种全部由碳六元环构成的新型二维碳纳米材料.从2004年发现至今,其在能源、电子、复合材料、生物医学等领域中的应用都取得了重大研究进展.近年来,石墨烯在分析化学领域也表现出了巨大的应用潜力,尤其是在环境有机污染物分析方面,涌现了大量相关报道.本文简要回顾了近期石墨烯在环境有机污染物分析中的应用情况,涵盖了样品前处理、色谱、传感器、质谱等不同的技术方向,并对石墨烯在环境分析中的应用前景进行了展望.     

鱼体中有机微污染物的定量及筛查研究进展

化学品通过多种途径进入环境水体,可对水生生物及人体健康造成潜在风险.鱼类作为水环境污染物监测的指示生物,分析鱼体内有机微污染物的分布特征是评估水环境安全的重要方法.现有污染物种类繁多,且在生物体内存在降解转化的过程,基于靶向定量分析的监测方法难以系统、准确地评估鱼体中有机污染物的暴露特征.由于具有高分辨率、高质量精度、...     

Discovery of emerging organic pollutants in the atmosphere through an omics approach

● We review the framework of discovering emerging pollutants through an omics approach. ● High-resolution MS can digitalize atmospheric samples to full-component data. ● Chemical features and databases can help to translate untargeted data to compounds. ● Biological effect-directed untargeted analyses consider both existence and toxicity. Ambient air pollution, containing numerous known and hitherto unknown compounds, is a major risk factor for public health. The discovery of harmful components is the prerequisite for pollution control; however, this raises a great challenge on recognizing previously unknown species. Here we systematically review the analytical techniques on air pollution in the framework of an omics approach, with a brief introduction on sample preparation and analysis, and in more detail, compounds prioritization and identification. Through high-resolution mass spectrometry (HRMS, typically coupled with chromatography), the complicated environmental matrix can be digitalized into “full-component” data. A key step to discover emerging compounds is the prioritization of compounds from massive data. Chemical fingerprints, suspect lists and biological effects are the most vital untargeted strategies for comprehensively screening critical and hazardous substances. Afterward, compressed data of compounds can be identified at various confidence levels according to exact mass and the derived molecular formula, MS libraries, and authentic standards. Such an omics approach on full-component data provides a paradigm for discovering emerging air pollutants; nonetheless, new technological advancements of instruments and databases are warranted for further tracking the environmental behaviors, hence to evaluate the health risk of key pollutants.     

大气中持久性有机污染物在气相和颗粒相中的分配特征研究进展

大气中持久性有机污染物(POPs)的气(气相)-粒(颗粒相)分配是影响POPs在大气中分布、迁移和转化的一个重要因素,研究POPs的气-粒分配特征有助于提高POPs环境归趋预测的准确性,对区域范围内的大气POPs污染防治具有重要意义.本文简要介绍了两种经典的POPs气-粒分配理论及模型,总结了有关大气中几类典型POPs在气相和颗粒相中的分配特征研究的最新进展,讨论了不同种类POPs气-粒分配的一些差异性特征和可能的影响因素,并提出了大气中新型POPs气-粒分配特征研究中亟待解决的问题.     

环境微塑料与有机污染物的相互作用及联合毒性效应研究进展

环境微塑料可吸附有机污染物,并与有机污染物进行相互作用从而改变其毒性效应,增加微塑料的治理难度.本文就全球范围内微塑料与有机污染物的相互作用及毒性效应的研究进展进行综述,分析不同介质中微塑料与有机污染物的共存水平、吸附机理、影响因素以及联合毒性效应等.研究表明,微塑料可作为多环芳烃(PAHs)、多氯联苯(PCBs)、六...     

Sampling and analysis by GC/MS of the chitin synthesis inhibitors lufenuron and teflubenzuron in soil and soil invertebrates

A method for the measurement of benzoylphenyl ureas in soil, carabid beetles and earthworms was developed. These insecticides were transformed into their corresponding aniline derivatives in a hydrolytic step and subsequently measured by gas chromatography/mass spectrometry.     

Fabrication of highly efficient Bi2WO6/CuS composite for visible-light photocatalytic removal of organic pollutants and Cr(VI) from wastewater

• A novel Bi₂WO₆/CuS composite was fabricated by a facile solvothermal method. • This composite efficiently removed organic pollutants and Cr(VI) by photocatalysis. • The DOM could promoted synchronous removal of organic pollutants and Cr(VI). • This composite could be applied at a wide pH range in photocatalytic reactions. • Possible photocatalytic mechanisms of organic pollutants and Cr(VI) were proposed. A visible-light-driven Bi₂WO₆/CuS p-n heterojunction was fabricated using an easy solvothermal method. The Bi₂WO₆/CuS exhibited high photocatalytic activity in a mixed system containing rhodamine B (RhB), tetracycline hydrochloride (TCH), and Cr (VI) under natural conditions. Approximately 98.8% of the RhB (10 mg/L), 87.6% of the TCH (10 mg/L) and 95.1% of the Cr(VI) (15 mg/L) were simultaneously removed from a mixed solution within 105 min. The removal efficiencies of TCH and Cr(VI) increased by 12.9% and 20.4%, respectively, in the mixed solution, compared with the single solutions. This is mainly ascribed to the simultaneous consumption electrons and holes, which increases the amount of excited electrons/holes and enhances the separation efficiency of photogenerated electrons and holes. Bi₂WO₆/CuS can be applied over a wide pH range (2–6) with strong photocatalytic activity for RhB, TCH and Cr(VI). Coexisiting dissolved organic matter in the solution significantly promoted the removal of TCH (from 74.7% to 87.2%) and Cr(VI) (from 75.7% to 99.9%) because it accelerated the separation of electrons and holes by consuming holes as an electron acceptor. Removal mechanisms of RhB, TCH, and Cr(VI) were proposed, Bi₂WO₆/CuS was formed into a p-n heterojunction to efficiently separate and transfer photoelectrons and holes so as to drive photocatalytic reactions. Specifically, when reducing pollutants (e.g., TCH) and oxidizing pollutants (e.g., Cr(VI)) coexist in wastewater, the p-n heterojunction in Bi₂WO₆/CuS acts as a “bridge” to shorten the electron transport and thus simultaneously increase the removal efficiencies of both types of pollutants.     

Organic pollutants in riparian wetlands of the Lippe river (Germany)

Organic-geochemical investigations were performed on layers of a dated sediment core taken from a riparian wetland of the Lippe river, Germany. The samples were collected from two distinct depth intervals representing sedimentation periods of 1944–1952 and 1972–1984, respectively. Comprehensive screening analyses by gas chromatography-mass spectrometry (GC-MS) revealed a complex mixture of anthropogenic contaminants. Here, we report the quantitative distribution of selected persistent lipophilic organic substances characterizing municipal as well as industrial emissions. Considering both geochemical and geochronological data, we deduced time-dependent information about industrial production and domestic effluents for the region investigated. In addition, usage and subsequent emission of characteristic pollutants into the riverine system were interpreted for both time periods monitored.