土壤、沉积物和植物样品中多环芳烃（PAHs）不同提取与净化方法比较

系统分析和比较了土壤、沉积物和植物样品中多环芳烃（PAHs）的提取与净化方法,阐述和对比了索氏提取法、超声波提取法、超临界流提取法、固相提取与固相微提取法、固液提取法、微波辅助提取法、快速溶剂提取法等提取方法以及定量浓缩净化法、硅胶柱层析净化法、费罗里土柱层析净化法、氧化铝净化法、固相萃取（SPE）净化法等净化方法。旨在通过比较目前的提取和净化方法,展望将来提取与净化方法发展的新方向。     

底泥中多环芳烃（PAHs）提取方法评析

总结了底泥中多环芳烃（PAHs)提取的处理流程和国内外多种提取方法，比较了几种在我国较为常用的提取方法的效率，同时还提出了PAHs分离纯化的方法和步骤，并指出了提取过程中影响实验回收率的几个因素。     

土壤多环芳烃生物可给性测定的体外胃肠模拟法研究进展

经口摄入是土壤多环芳烃(PAHs)人体暴露的重要途径, 有效评估土中PAHs的生物可给性是全面评估土壤PAHs人体健康风险的重要组成部分。然而, 测定土壤PAHs生物可给性的体外胃肠模拟方法众多, 至今国内外尚缺乏统一标准。由于不同体外模拟方法测定的结果差异较大, 制约了土壤PAHs人体健康风险评估的发展。基于此, 本文综述了PAHs生物可给性测定所用的多种体外胃肠模拟方法及进展, 并针对PAHs生物可给性测定方法存在的问题, 建议未来构建土壤PAHs生物可给性测定标准方法的相关研究应从生理条件、吸附材料的选择、体内模型的验证这三方面综合考虑。综合以上，本文有望对我国污染场地土壤标准体系构建和完善、前瞻性科学管理提供科学依据。     

中国优控多环芳烃土壤污染特征及国内外生物可给性研究进展

多环芳烃(Polycyclic aromatic hydrocarbons,PAHs)是一类持久性有机污染物,容易在土壤中累积并且毒性显著,但PAHs在土壤固相上的吸附性较强,基于土壤污染总量暴露会导致高估人群健康风险。本研究基于2000-2020年间发表的123篇文献,总结了我国土壤中16种优先控制多环芳烃(∑16PAHs)的污染浓度分布和组成特征,介绍了11种常见的模拟PAHs生物可给性测试方法和主要影响因素,并总结了PAHs的生物可给性系数范围。研究结果表明土壤∑16PAHs最高与平均浓度分别为23 250 和1 314.7 μg.kg-1污染较为严重;近年来PAHs生物可给性测试方法主要基于生理原理提取法(PBET),在模拟消化过程和吸附剂等方面不断完善和改进,并且消化条件、土壤性质等因素对生物可给性结果影响较大。16种PAHs的生物可给性平均值范围为13.2%~72.4%,其中?和苯并[b]荧蒽的生物可给性较高,对∑16PAHs暴露产生贡献较高。本研究为开展土壤PAHs污染精细化风险评估研究提供重要理论参考依据。     

食品中挥发性风味成分提取技术研究进展

挥发性成分提取技术是食品风味分析的基础,本文分别介绍了溶剂萃取法、蒸馏法、顶空捕集法和吸附剂萃取法4类食品中挥发性风味成分的提取方法及其在食品中的应用与优缺点,重点阐述了吸附萃取法中的固相微萃取和搅拌棒吸附萃取技术,以期为食品中挥发性风味成分的研究提供参考。     

土壤养分有效性测定及其方法

在提出土壤养分有效性测定概念的基础上 ,本文对各种土壤养分有效性的测定方法进行了总结 ,讨论了这些方法的测定机理、测定效果及近几年的进展。这些方法包括用于磷钾等元素测定的树脂法、用于氮测定的生物培养法和化学提取法、磷测定的氧化铁试纸法和氢氧化铁透析管法和钾的四苯硼钠法     

红叶李花中总黄酮提取工艺及抑制α-葡萄糖苷酶活性研究

为进一步开发红叶李资源,筛选其活性成分,通过比较水煮沸、醇回流、超声、微波、闪式、超临界CO_2(SFE-CO_2)、复合酶酶解等提取方法对红叶李花中总黄酮含量的影响和对α-葡萄糖苷酶活性的抑制效果,确定最佳提取方法,并通过单因素试验和响应面法优选提取工艺。结果表明,复合酶酶解联合SFE-CO_2萃取工艺提取效率和生物活性最佳,SFE-CO_2萃取的总黄酮对α-葡萄糖苷酶抑制率达到96.09%,IC50为12.16μg·m L-1。最佳提取工艺为:酶解温度30℃,酶解时间3.5 h,酶用量0.10%,萃取压力30 MPa,乙醇浓度85%,萃取温度45℃,萃取时间60 min。此条件下的总黄酮得率为11.55%。本研究结果为红叶李花中总黄酮的开发与利用提供了技术参考。     

胭脂萝卜红色素提取的原理和方法

胭脂萝卜红色素是一种具有优势的天然红色素。介绍了该红色素的结构,综合前人研究成果,分析讨论了有机溶剂提取法、水浸提法、大孔吸附树脂法、酶工程技术法、高速分离法等提取方法．认为今后的研发重点是如何使一些新兴的技术如超临界流体萃取技术(SFE)、超滤技术(UF)、酶工程技术等工业化、普及化。     

乌鲁木齐市周边地区土壤中多环芳烃的含量及来源

在乌鲁木齐市周边,从乌拉泊到水西沟按不同距离与深度进行土壤样品采集,采用索氏提取法与层析净化法进行预处理,高效液相色谱法测定土壤中16种多环芳烃(PAHs)的含量,并对PAHs进行对比分析、污染评价和来源分析的相关研究。结果表明:总PAHs平均浓度为998.23(306.94~3 652.16)ng/g,污染程度差异不大,处中度污染水平但更接近严重污染水平;16种PAHs的最低检测限为0.20~0.80 ng/g;一些采样点的表层土壤中苯并[a]芘的含量高于土壤质量控制标准。不同层次土壤PAHs的污染程度有所不同,其顺序为表层中层下层;高分子量(4~6环)PAHs占据了总含量的84.1%,低分子量(2~3环)PAHs占据15.9%,得出在乌鲁木齐市周边土壤中PAHs的重要来源是汽车排放,同时煤燃烧排放的贡献也很大。     

应用于环境中有机污染物分析的一些新技术

本简述了近年来研究较多的快速检测技术，免疫检测法、传感器，及色谱的一些新发展，还讨论了固相萃取，超临界流体萃取，免疫亲合色谱提取净化的方法及其新进展。     

Procedure to measure the level of polycyclic aromatic hydrocarbons in wood ashes used as fertilizer in agroforestry soils and their transfer from ashes to water

Before wood ash can be safely used as a fertilizer in soils, possible negative effects such as input of organic contaminants or remobilization of contaminants already stored in the soil must be investigated. The objective of this study was to optimize and characterize extraction methods to isolate and quantitatively measure polycyclic aromatic hydrocarbons (PAHs) concentrations in wood ash that can be used as amendment of soils. It will be then possible to examine the effects of wood ash application on PAHs concentrations in the washing waters with the aim of evaluating their distribution by storage in the different compartments and what influences their stability and persistence. Simple, rapid and inexpensive methods have been set up for the determination of seven polycyclic aromatic hydrocarbons (PAHs) in wood ashes and ash aqueous extracts without interferences from other chemical contaminants using organic solvent extraction and/or SPE techniques and analyzed by an optimized RP-HPLC-FLD method. The feasibility of extraction for the determination of PAHs in wood ashes has been evaluated because PAHs are strongly sorbed to such a matrix, which explains why the PAHs content in ash was seldom studied. The method resulted to be of recoveries ranging from 81 to 97% for the different PAHs, with repeatabilities (RSDs%) better than 6%. Detection levels were from 0.2 to 2.2 microg/kg, while quantification limits were from 0.7 to 5.6 microg/kg, low enough to evaluate the presence of PAHs in wood ashes.     

Comparison of strategies for extraction of high molecular weight polycyclic aromatic hydrocarbons from drinking waters

Simple, rapid, and inexpensive methods have been developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in drinking waters without interferences from other chemical contaminants by use of two different extraction techniques and analysis by an optimized reverse-phase (RP) high-performance liquid chromatography followed by fluorescence detection (HPLC-FLD) method. The feasibility of SPE (solid-phase extraction) and SPME (solid-phase microextraction) for the determination of PAH in drinking water samples has been evaluated. Several parameters have been studied and optimized for both extraction procedures. The relationship between the nature of the fibers and the quantity of extracted compounds and the effects of organic solvent, salt addition, sampling temperature, and sampling time was studied for SPME. Acetonitrile percentage added to the sample, sample storage conditions (temperature and time), and type of organic elution solvent and elution volume were evaluated for SPE. The results show that both extraction procedures can be used to determine PAHs in drinking waters, but SPE gives better performance (recovery, precision, and quantification limits) for the determination of PAHs in drinking water at the levels established by the legislation.     

Investigation of sample treatment steps for the analysis of polycyclic aromatic hydrocarbons in ground coffee

Sample treatment procedures were tested for the determination of polycyclic aromatic hydrocarbons (PAHs) in ground coffee. Pressurized liquid extraction (PLE), under different conditions, was combined with several cleanup methods, namely in situ purification, C18-silica solid-phase extraction (SPE), silica SPE, acid digestion, and alkaline saponification. Soxhlet extraction and direct alkaline saponification were also tested. Best results were obtained using PLE with hexane/acetone 50:50 (v/v) under 150 degrees C. Alkaline saponification followed by cyclohexane extraction and silica SPE was required to eliminate interferent compounds. Finally, 11 PAHs could be quantified in ground coffee with limits of detection in the range of 0.11-0.18 microg kg(-1). Application to ground Arabica coffee lots from Colombia revealed the presence of several PAHs, giving an overall toxicity equivalence in the range of 0.16-0.87 microg kg(-1). PAH identification was performed using both high-performance liquid chromatography-diode array detection and gas chromatography coupled to mass spectrometry.     

Accelerated solvent extraction and gas chromatography/mass spectrometry for determination of polycyclic aromatic hydrocarbons in smoked food samples.

Accelerated solvent extraction (ASE) is a new sample extraction method offering a number of advantages such as low pe -extraction cost, reduced solvent and time consumption, and simplified extraction protocols. In this study, the ASE method was applied to the extraction of polycyclic aromatic hydrocarbons (PAHs) from biological samples. For recovery studies, fish tissues and ground pork were used as sample matrices. Sample aliquots fortified with 16 PAHs were extracted by ASE, and the extracts were treated with sulfuric acid and Florisil, followed by gas chromatography-mass spectrometry analysis. The PAH recoveries by the ASE method were found to be comparable with or better than those by Soxhlet extraction. The extraction and quantitation method was then applied to the determination of PAHs in several smoked meat samples obtained from a local market. Up to 12 PAHs were found to be present at concentrations ranging from 3 to 52 ng/g wet sample.     

Estimation of PAH bioavailability to Lepidium sativum using sequential supercritical fluid extraction – a case study with industrial contaminated soils

For the determination of PAH availability to plants a plant accumulation test with Lepidium and sequential supercritical fluid extraction (SSFE) with carbon dioxide as extraction solvent was used, during which the extraction conditions were changed from mild to harsh in order to represent a broad range of potential pollutant-soil interactions. Both approaches were applied in laboratory experiments on industrial contaminated soils which, in addition, were also freshly spiked with PAHs in order to increase the bioavailability. Only Naphthalene, Phenanthrene and, in some cases, Pyrene accumulated from the industrial contaminated soils. Accumulation experiments with spiked industrial soils showed that other PAHs, for example Anthracene, Fluorene and even high weight PAHs like Benzo(a)pyrene, also could be taken up by plants. SSFE extraction data were compared to accumulated amounts of PAHs in the plants. Strong correlations were found for Phenanthrene between plant accumulation and extractability under very mild extraction conditions. For Naphthalene, accumulation did not correlate with its extractability in the industrial soils. The possibility exists that bioavailability in soil was eclipsed by an accumulation in the gas phase due to the high volatility of Naphthalene. Supercritical fluid extraction appears to be a promising tool to estimate Phenanthrene availability to plants, but further studies for the evaluation of other PAHs are recommended. This could be helpful for the determination of the feasibility of phytoremediation applications on industrially contaminated soils.     

Determination of parent and substituted polycyclic aromatic hydrocarbons in high-fat salmon using a modified QuEChERS extraction, dispersive SPE and GC-MS

A fast and easy modified QuEChERS (quick, easy, cheap, rugged and safe) extraction method has been developed and validated for determination of 33 parent and substituted polycyclic aromatic hydrocarbons (PAHs) in high-fat smoked salmon that greatly enhances analyte recovery compared to traditional QuEChERS procedures. Sample processing includes extraction of PAHs into a solution of ethyl acetate, acetone and isooctane followed by cleanup with dispersive SPE and analysis by GC-MS in SIM mode. Method performance was assessed in spike recovery experiments (500 μg/g wet weight) in three commercially available smoked salmon with 3-11% fat. Recoveries of some 2-, 3- and 5-ring PAHs were improved 50-200% over traditional methods, while average recovery across all PAHs was improved 67%. Method precision was good with replicate extractions typically yielding relative standard deviations <10%, and detection limits were in the low ng/g range. With this method, a single analyst could extract and clean up ≥60 samples for PAH analysis in an 8 h work day.     

Polycyclic aromatic hydrocarbon profile analysis of high-protein foods, oils, and fats by gas chromatography.

A method is described for the determination of polycyclic aromatic hydrocarbons (PAHs) with 3-7 rings in (I) meat, poultry, fish, and yeast; and (II) oils and fats. The extraction of PAHs from group I is incomplete, and, therefore, group I samples must be dissolved homogeneously by saponification in 2N methanolic potassium hydroxide. The PAHs are concentrated by liquid-liquid extraction (methanol-water-cyclohexane, N,N - dimethylformamide - water-cyclohexane) and by column chromatography on Sephadex LH 20. The PAHs are separated by high-performance gas-liquid chromatography (GLC) with columns containing 5% OV-101 on Gas-Chrom Q and estimated by integration of the flame ionization detector signals in relation to an internal standard (3,6-dimethylphenanthrene and/or benzo(b)chrysene). The sensitivity is significantly higher than that obtained with ultraviolet spectroscopic methods. The reproducibility and margin of error were tested with meat samples fortified with 11 PAHs and with samples of sunflower oil. The method was further applied to meat, smoked fish, yeast, and unrefined sunflower oil. All samples investigated contained more than 100 PAHs (characterized by mass spectrometry) of which only the main components were determined: phenanthrene, anthracene, fluorene, fluoranthene, pyrene, benzo(a)anthracene, chrysene, benzo(b)fluoranthene + benzo (j)fluoranthene + benzo(k) fluoranthene, benzo(e)pyrene, benzo(a)pyrene, perylene, dibenz(a,j)anthracene, dibenz(a,h)anthracene + indeno(1,2,3,-cd)pyrene, benzo(ghi)perylene, anthanthrene, and coronene. In contrast to other methods, the GLC profile analysis allows the recording of known and unknown PAH peaks simultaneously and also allows a compilation of all PAHs.     

生物质炭中多环芳烃的潜在环境风险研究进展

作为土壤改良剂和环境污染修复材料,生物质炭在近年来得以广泛应用。生物质炭制备过程中会产生一定量的多环芳烃(PAHs),对其潜在环境负面效应和风险尚缺乏应有的认识。本文总结了生物质炭中PAHs的形成机理、影响因素(包括原材料、裂解温度、裂解升温速率和保留时间等)、总量和生物有效含量及其分析方法,旨在为生物质炭在环境中的安全应用提供理论依据和技术参考。     

Prediction of Polycyclic Aromatic Hydrocarbon Bioaccessibility to Earthworms in Spiked Soils by Composite Extraction with Hydroxypropyl-β-Cyclodextrin and Organic Acids

Traditional exhaustive extraction methods often overestimate the risk of polycyclic aromatic hydrocarbon(PAH) bioaccessibility to biota. Therefore, reliable assessment methods need to be established. In this study, a composite extraction with hydroxypropyl-β-cyclodextrin(HPCD) and three low-molecular-weight organic acids, oxalic acid(OA), malic acid(MA), and citric acid(CA), was used to predict the PAH bioaccessibility to earthworms, subjecting to two soils(red soil and yellow soil) spiked with selected PAHs,phenanthrene, pyrene, chrysene, benzo(a)anthracene, benzo(b)fluoranthene, benzo(k)fluoranthene, and benzo(a)pyrene. For both soils,concentrations of PAHs by composite extraction using HPCD-OA(R~2= 0.89–0.92, slope = 1.89–2.03; n = 35), HPCD-MA(R~2=0.92–0.96, slope = 1.43–1.67; n = 35), and HPCD-CA(R~2= 0.92–0.96, slope = 1.26–1.56; n = 35) were significantly correlated with PAH accumulation in the Eisenia fetida earthworms. Moreover, the HPCD-CA-and HPCD-MA-extracted PAH concentrations were closer to the earthworm-accumulated PAH concentration than the extraction using just HPCD. The results indicated that the composite extraction could improve the prediction of PAH bioaccessibility, and therefore can serve as a reliable chemical method to predict PAH bioaccessibility to earthworms in contaminated soils.