Packed in-tube solid phase microextraction with graphene oxide supported on aminopropyl silica: Determination of target triazines in water samples

On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2–4.0 µg L^?1) and low detection limits (1.1–2.9 ng L^?1). The high extraction efficiency was determined with enrichment factors ranging from 1.2–2.9 for the lowest level, 1.3–4.9 intermediate level and 1.2–3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.     

植物释放挥发性有机物(BVOC)向二次有机气溶胶(SOA)转化机制研究

利用自制玻璃生态罩,研究植物挥发性有机物（BVOC）的释放机制.在紫外光诱导条件下,BVOC经历一系列的光氧化反应,最终产生了二次有机气溶胶（SOA）.运用固相微萃取（SPME）和气相色谱-质谱联用（GC-MS）技术,对目标植物（驱蚊草）释放出的BVOC进行采样分析,共检测出7种主要化合物,其中主要为单萜类、倍半萜类、醇类和酮类物质.研究发现,在紫外光的照射下,这些BVOC可以发生光氧化反应转化为SOA.利用串联差分淌度分析仪（TDMA）测定SOA的粒径分布和SOA颗粒物的吸湿性.结果表明粒径范围大致是50～320 nm,吸湿性研究发现这些SOA具有吸湿性,生长因子可以从1.05增长到1.11.     

大气低分子有机酸研究方法及其前沿问题

文章系统地阐述了大气有机酸的研究历史、现状和目前存在问题及可能取得研究进展的方法。低分子有机酸是大气中重要的微量挥发性有机碳组分,它们广泛存在于大气对流层中,对气候、环境和生态系统具有重要影响。长期以来,对大气有机酸的研究都是基于其含量的分析,尽管这一研究手段对有机酸的认识起到了推动作用,但含量的分析已越来越不能满足于当前人们对大气有机酸生物地球化学认识的需求。由于稳定同位素组成的示踪作用,近年来人们开始探索利用有机酸中碳同位素的测试分析方法来研究其循环过程。这一方法涉及水溶液中有机酸的萃取过程。由于其近发、半挥发性和其易污染性,常规的萃取方法不能应用于有机酸的萃取。最近出现的固相微萃取技术为有机酸碳同位素组成的准确分析研究提供了可能的途径。利用这一方法探索有机酸同位素组成的分析,有可能为大气有机酸生物地球化学循环研究开辟一片新的天地,从而使该领域研究向前推进一步。     

固相微萃取-气质联用法测定水中痕量土臭素和二甲基异崁醇

采用固相微萃-气相色谱/质谱法(SPME-GC/MS)对GSM和2-MIB进行富集检测。实验对萃取富集和仪器条件进行了优化,得出最佳实验条件：NaCl投加量30%,萃取温度65℃,萃取时间40 min,解吸3 min,不分流进样,SIM模式采集数据。实验还对萃取头的使用次数和维护进行了探讨。利用已经建立的SPME-GC/MS法对佛山市28家水厂的出厂水和原水、佛山典型景观千灯湖和亚艺公园湖水进行普查。该法具有操作简单快速、能实现自动化连续检测、准确、灵敏度高等特点,适用于饮用水中嗅味物质定性和定量。     

Evaluation of pesticides multiresidue contamination of khat leaves from Jazan region,Kingdome Saudi Arabia,using solid-phase extraction – gas chromatography/mass spectrometry

The habit of khat chewing is widespread with a deep-rooted sociocultural tradition in these regions and as such poses a public health problem. The use of pesticides is considered to be indispensable practice for the production of adequate food supply for the increasing demands by the global population and for control of insect-borne diseases. Thus, contamination of the environment with pesticides and entry of these chemicals into the food chain is unavoidable especially in developing countries. The main objective of our current study was to assess pesticide pollution of khat leaves (unknown origin) obtained while being smuggled into the Kingdom of Saudi Arabia and to be used in Jazan area. A total of 120 khat leaf samples were extracted using solid-phase extraction followed by gas chromatography/mass spectrometry analysis for the presence of 69 standard pesticides using an internal standard, tiphenyl phosphate. No pesticide residues were detected in all the studied samples. These data as preliminary and more experiments need to be performed to confirm our present findings. Routine monitoring of the pesticide residues is important for the prevention, control, and reduction of environmental pollution and also for legal decisions to minimize health risks.     

Matrix effect on the performance of headspace solid phase microextraction method for the analysis of target volatile organic compounds (VOCs) in environmental samples

Solid phase microextraction (SPME) is a fast, cheap and solvent free methodology widely used for environmental analysis. A SPME methodology has been optimized for the analysis of VOCs in a range of matrices covering different soils of varying textures, organic matrices from manures and composts from different origins, and biochars. The performance of the technique was compared for the different matrices spiked with a multicomponent VOC mixture, selected to cover different VOC groups of environmental relevance (ketone, terpene, alcohol, aliphatic hydrocarbons and alkylbenzenes). VOC recovery was dependent on the nature itself of the VOC and the matrix characteristics. The SPME analysis of non-polar compounds, such as alkylbenzenes, terpenes and aliphatic hydrocarbons, was markedly affected by the type of matrix as a consequence of the competition for the adsorption sites in the SPME fiber. These non-polar compounds were strongly retained in the biochar surfaces limiting the use of SPME for this type of matrices. However, this adsorption capacity was not evident when biochar had undergone a weathering/aging process through composting. Polar compounds (alcohol and ketone) showed a similar behavior in all matrices, as a consequence of the hydrophilic characteristics, affected by water content in the matrix. SPME showed a good performance for soils and organic matrices especially for non-polar compounds, achieving a limit of detection (LD) and limit of quantification (LQ) of 0.02 and 0.03 ng g⁻¹ for non-polar compounds and poor extraction for more hydrophilic and polar compounds (LD and LQ higher 310 and 490 ng g⁻¹). The characteristics of the matrix, especially pH and organic matter, had a marked impact on SPME, due to the competition of the analytes for active sites in the fiber, but VOC biodegradation should not be discarded in matrices with active microbial biomass.     

固相微萃取-气相色谱法测定水源地水中SVOC

采用固相微萃取-毛细管柱电子捕获气相色谱法测定水源地水中18种半挥发性有机物,优化了萃取纤维、时间、温度、pH值、转子转速、离子强度等萃取条件。方法线性良好,18种化合物的检出限为0.000 2μg/L~0.1μg/L,实际水样加标回收率为84.3%~109%。     

固相微萃取分析条件的优化

主要介绍了固相微萃取作为一种样品前处理技术，如何对影响其分配系数的各因素，如：萃取头的选择、萃取方式、萃取温度等进行优化选择，从而提高方法灵敏度及回收率。     

固相微萃取-毛细管气相色谱法快速同步分析水中有机氯及有机磷农药

固相微萃取是一种快速、简便,集萃取浓缩进样于一体的样品前处理技术,具有分析时间短、灵敏度高、无需有机溶剂的优点.用固相微萃取富集水中8种有机氯及7种有机磷农药,毛细管气相色谱ECD检测器分离分析,整个分析过程只需26min,检出限可达0.002～1μg/L,已用于地表水中有机氯及有机磷农药含量的测定.     

Headspace-SPME-GC-MS Identification of Volatile Organic Compounds Released from Expanded Polystyrene

A method for the identification of volatile organic compounds (VOCs) released from packaging expanded polystyrene (EPS) is presented. Headspace solid-phase microextraction (HS-SPME) with a 75-m carboxen-polydimethylsiloxan fiber was used as sample preparation technique before the determination of the volatile organic compounds by gas chromatography–mass spectrometry (GC-MS). For separation of compounds, two fused silica capillary columns of different polarity (DB-5ms and BPX-50) were used. Styrene monomer with his impurities and oxidation products, as well as residual pentane, were identified in the headspace of EPS.