长期施用鸡粪对土壤重金属积累的影响与评价

研究了金华市郊长期施用规模化养殖场鸡粪的蔬菜基地土壤重金属的积累现状.结果表明,该基地土壤重金属(Pb、Cd、Cu、Cr)含量已有一定程度的积累,其中80%大棚土壤已处于污染警戒水平(2级).其中,单一元素Cd污染严重,80%的基地土壤重金属镉含量已达轻度污染程度;其他元素含量虽未超标,但都有一定程度的积累.     

火焰原子吸收光谱法测定山野菜刺嫩芽中钙镁铁锰

随着人们对纯自然、无污染、无农药和化肥的绿色食品的渴望和需求，山野菜已成为城市人喜食的美味佳肴。刺嫩芽是众多山野菜中的一种，俗称“刺龙芽”“刺老鸦”，生长于山区，属无污染天然绿色食品。     

赣南中药材基地土壤微量元素含量评价

对赣南中药材基地土壤微量元素含量状况的统计分析表明,该区土壤有效态微量元素含量丰富,依据全国微量元素分级标准,中药材基地土壤有效锰多为Ⅱ级,占总样数71.87%;有效锌多处于Ⅰ级或Ⅱ级,占总样数96.88%,其中褐土均为Ⅰ级;土壤有效铜有3个土样处于Ⅱ级,其余均为Ⅰ级;土壤有效铁均处于Ⅰ级或Ⅱ级,褐土Ⅰ级较多,占总样数18.75%,黄棕壤Ⅱ级较多,占总样数28.13%。     

无公害蔬菜、灌溉水、种植土壤中Pb、As、Cd、Cr的测定

采用原子吸收光谱法测定了广西区内几个无公害生产基地土壤、蔬菜、水样中Pb、As、Cd、Cr的含量,RSD＜7％,回收率在94％－110％之间。用本法测定GBW 08302土壤标准物质,测得值与推荐值基本一致。     

火焰原子吸收光谱法测定食用花卉中铁、锌、钙、镁

随着“绿色食品”及恢复“自然食物”的风气日盛，食花成为新时尚，有专家预言花卉将成为22世纪新的人类食物源。     

外源稀土对土壤微生物特征的影响及时间效应

采用微生物生物量、Cmic/Corg、呼吸速率、代谢熵qCo2及BIOLOG等方法分析稀土对土壤微生物活性及群落结构的影响和时间效应。结果表明，低浓度稀土进入土壤的早期阶段对土壤微生物具有刺激作用，但随时间的推移逐渐不显著。高浓度稀土对土壤微生物具有抑制作用，随时间的延长有减少的趋势。BIOLOG分析显示，稀土施用之后，土壤微生物对碳源的消耗量增加，速度加快，群落结构发生了改变且具有长期性。     

电感耦合等离子体质谱法测定绿色食品中15种稀土元素

本文用电感耦合等离子体质谱法测定了绿色食品(主要包括大米、茶叶、纯净水)中15个稀土元素；考察了基体元素Cl、Na、Ca、C的基体效应及校正方法，确定了仪器最佳工作参数。方法的检出限为0．03～0．13μg／L，相对标准偏差为0．2％～10．8％。     

土壤环境生态对重金属元素迁移影响分析

作物中重金属元素主要来自土壤，其含量与作物种类和土壤环境有关。土壤中重金属元素含量、土壤pH值、Eh值、土壤化学组成、土壤质地等环境因素都影响作物中重金属元素含量。土壤pH值和Eh值影响重金属元素的活动性。重金属元素的水溶态容易被作物吸收，而难溶态和被土壤胶体固定的重金属元素，不能被作物吸收。同种作物重金属元素含量的差异主要取决于土壤环境。     

土壤环境中的硒对人和动物健康的影响

硒是人和动物必需的微量元素之一。土壤中的硒含量过多或过低，人和 动物都会出现地方性疾病。土壤中硒的含量与土壤母质、地形、气候条件和土壤条件性质等有关，调节土壤性质可以改善作物的含硒量。防治硒缺额症和硒中毒症，每天必需摄入适量的硒，以100－200μg为宜，但人体对硒的需要量也与食物成分有关。     

稀土在土壤中运移数值模拟研究

９种不同性质土壤Ｃｅ和Ｎｄ吸附和度达５０％时，用同位素示踪法和数值模拟法对ＲＥ运移进行比较，发现两者对极大多数土壤有较好的拟合性。说明该数值模拟程序对预测稀土长期在土壤中运移具有一定的可靠性。预测结果表明，在自然降雨量情况下，ＲＥ吸附饱和度１０％时，在吸附容量小的酸性土壤中，ＲＥ下移约每年１ｃｍ，吸附容量中等的中性、策酸性土壤，每两年约下移１ｃｍ而吸附容量较大的碱性土壤，ＲＥ很难被雨水运移。     

Determination of polar nitroaromatic compounds in soils and the impact of the soil properties on the extraction results

An HPLC compatible method based on pressurized solvent extraction (PSE) for the determination of fifteen polar nitroaromatic compounds (pNC) in soil is described. The PSE method was compared with ultrasonic activated extraction. Thereby, analyzing sandy, clayey, and organic rich spiked soil samples, the influence of soil texture on the extraction yield was examined. Considering different soil properties recovery rates of investigated pNC and limiting extraction parameters were determined for both techniques. The extraction recovery of some pNC was found to show dependence on the clay content and correlation with the organic carbon amount of the soil.     

合成钛硅分子筛TS-1的一种新方法

In both conventional method[1] and modified method[2] ,organic Si and Ti alkoxides were used as Si source and Ti source respectively, and only strong organic base was used. So this system may be called as organic synthesis one (see Fig 1 )Thangaraj et al[3] reported that in the organic synthesis system only organic strong base TPAOH can be used.     

基于QuEChERS-HPLC法检测油炸食品中丙烯酰胺的含量

建立了基于QuEChERS(quick,easy,cheap,effective,rugged and safe)-HPLC测定油炸食品中丙烯酰胺含量的方法。 该方法的优势在于：改进的QuEChERS前处理方法中没有引入有机溶剂而直接采用纯水消除样品基底的影响。 研究中,使用纯水超声提取丙烯酰胺,丙基乙二胺(PSA)吸附剂分散净化提取液,乙腈和水(体积比1∶99)作为流动相,水系C18色谱柱分离,208 nm紫外波长条件下检测丙烯酰胺的含量。 结果表明,丙烯酰胺在0.020~0.800 μg/g浓度范围内与出峰面积呈线性关系,相关系数r=0.9994;检测限为0.005 μg/g;加标回收率为83.96%~89.43%,相对标准偏差(RSD)为2.13%~5.87%。 该方法具有操作简单、快速、可靠和灵敏度高等特点,成功应用于方便面等油炸食品中丙烯酰胺含量的测定。     

重金属有效态与土壤环境质量标准制订

制订合适的土壤环境质量标准是评价土壤健康质量及食品安全的核心问题,而土壤重金属有效态对制定土壤环境质量标准具有重要意义。土壤重金属有效态主要指植物有效态,它与重金属形态关系密切。影响土壤重金属有效态的因素很多,主要包括:土壤pH值、氧化还原电位、CEC、有机质含量、粒径组成(黏粒含量)、铁铝锰氧化物含量、植物种类、土壤微生物、土壤温度的高低、重金属来源等。化学试剂浸提法是测量重金属生物有效性的常用方法,所用化学试剂主要有三类:弱(稀)酸、络合剂和中性盐,中性盐由于对土壤pH值影响小而受到重视。我国现行土壤质量标准采用土壤重金属总量和pH两个因素为依据,但是不少学者认为,该标准仅适用于重金属有效态较高的土壤,而不能反映重金属有效态含量较低土壤的实际状况。     

顶空气相色谱法测定食品添加剂中15种有机溶剂残留量

建立了顶空气相色谱法同时测定食品添加剂中甲苯、甲醇、正己烷等15种有机溶剂残留量的分析方法。选择N,N-二甲基甲酰胺对不同食品添加剂中的有机溶剂进行提取,将样液转移至顶空瓶中密封,顶空进样测定。对提取溶剂、提取方式、平衡时间和平衡温度等进行了优化。结果表明,15种有机溶剂分离良好,各残留溶剂在相应浓度范围内呈良好的线性关系,相关系数不小于0.999 8,定量下限为10.0 mg/kg(三氯甲烷和吡啶为20.0 mg/kg),回收率为90.6%~109.1%,相对标准偏差为0.1%~7.2%。该方法灵敏度高,重现性好,适用于食品添加剂中甲苯、甲醇、正己烷等15种残留溶剂的检测分析。     

Analysis of phenoxyalkanoic acid herbicides and their phenolic conversion products in soil by microwave assisted solvent extraction and subsequent analysis of extracts by on-line solid-phase extraction-liquid chromatography

A multiresidue method for the determination of phenoxyalkanoic acid herbicides and their phenolic conversion products in soil was developed. The method was based on microwave-assisted solvent extraction (MASE) of soil samples by an aqueous methanolic mixture and subsequent analysis of extracts by automated solid-phase extraction followed by on-line high-performance liquid chromatography and diode array detection. MASE parameters (extraction temperature and time, composition of the extraction mixture and extraction volume) were optimized with respect to analyte recoveries. The method was validated with two types of soils containing 1.5 and 3.5% organic matter, respectively, both types containing fresh and aged residues of sought analytes. Under the selected analytical conditions when soils with fresh residues were analyzed all target analytes were recovered above 80% from the soil containing 1.5% organic matter, while limits of identification at the level of 20-40 ng/g were achieved. From the soil containing 3.5% organic matter the least polar phenolic analytes exhibited slightly reduced recoveries, while identification limits of 30-50 ng/g were achieved. Samples with aged residues exhibited reduced recoveries for some analytes, the reduction amounting up to 6-12% within 1 month of aging period depending on soil organic matter.     

Quantitative EPR study on free radicals in the natural polyphenols interacting with metal ions and other environmental pollutants

Quantitative electron paramagnetic resonance (EPR) method was applied to characterise radicals stabilised in polyphenolic matrices of various biogenic materials: lichens, mosses, composts, soils, peats, brown coals and sewage sludge sediments. The investigations were carried out on raw materials and extracted fractions of humic acids (HA). General trends of g value and spin concentration changes were found. These parameters in lichens strongly depend on lichen species and air pollution. Determination of the g value and semiquinone spin concentration allows to assess degree of transformation of organic matter in compost, soil, peat and lignite. Application of gaseous ammonia as a base penetrating the organic matrices extends the possibilities and usefulness of the method. Interaction of metal ions with humic materials is illustrated by interaction of VO2+ ion with peat and lignite HA as well as demineralised (raw and carbonised) brown coal. Our investigations demonstrate that quantitative EPR is a rapid and effective monitoring method to study the influence of various environmental factors on substances containing polyphenolic matrices.     

Application of ultrasound-assisted extraction to the determination of contaminants in food and soil samples

The application of ultrasound-assisted extraction (UAE) to the sample preparation of environmental and food samples has increased in the last years. This technique has been used in the development of methods for the analysis of numerous contaminants, including organic compounds (pesticides, pharmaceuticals, polycyclic aromatic hydrocarbons, polyhalogenated flame retardants, etc.) and heavy metals. The aim of this work is to review the application of this extraction procedure to the analysis of contaminants in food and soil and the comparison of its use with other well-established extraction procedures. The advantages and disadvantages of this technique together with the possibility of coupling UAE with other analytical techniques will be also discussed.     

Determination of pesticides in soil by liquid-phase microextraction and gas chromatography-mass spectrometry

Trace amounts of pesticides in soil were determined by liquid-phase microextraction (LPME) coupled to gas chromatography-mass spectrometry (GC-MS). The technique involved the use of a small amount (3 microl) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The organic solvent was repeatedly discharged into and withdrawn from the porous polypropylene hollow fiber by a syringe pump, with the pesticides being extracted from a 4 ml aqueous soil sample into the organic solvent within the hollow fiber. Aspects of the developed procedure such as organic solvent selection, extraction time, movement pattern of plunger, concentrations of humic acid and salt, and the proportion of organic solvent in the soil sample, were optimized. Limits of detection (LOD) were between 0.05 and 0.1 microg/g with GC-MS analysis under selected-ion monitoring (SIM). Also, this method provided good precision ranging from 6 to 13%; the relative standard deviations were lower than 10% for most target pesticides (at spiked levels of 0.5 microg/g in aqueous soil sample). Finally, the results were compared to those achieved using solid-phase microextraction (SPME). The results demonstrated that LPME was a fast (within 4 min) and accurate method to determine trace amounts of pesticides in soil.     

Screening and Quantification of Organic Pollutants in Soil Using Comprehensive Two-dimensional Gas Chromatography with Time-of-flight Mass Spectrometry

The identification and quantification of organic compounds in leaching basin soil is important for the evaluation of soil pollution. In this study, a non-target screening strategy and a quantitative analytical method were developed based on the accelerated solvent extraction method followed by comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry. First, a screening method for potential risk compounds in soil samples was established, and the major compounds were screened under the conditions such as matching similarity, signal-to-noise ratio, and relative area ratio. Second, a quantitative method was further developed by internal calibration curves for 50 main organic pollutants in the soil samples, including 27 polycyclic aromatic hydrocarbons and their derivatives (PAHs), 10 phthalic acid esters, eight phenolic compounds, and five benzene derivatives. The quantitative procedure exhibited good selectivity, accuracy, precision, low limits of detection (0.03–1.02?ng/g), and quantification (0.1–3.0?ng/g) for all target compounds. Finally, the proposed strategy was applied to the soil samples that were collected from a leaching basin and polluted by electroplating wastewater. Abundant PAHs and phenolic compounds were detected in the topsoil sample, which were mainly released from the electroplating wastewater. The application of this multi-dimensional strategy in leaching basin soil samples can also be used for the assessment of organic pollution in other complex soil samples.