土壤中拟除虫菊酯类残留农药的气相色谱测定方法研究

建立了土壤中氯氰菊酯、氰戊菊酯和溴氰菊酯的提取、净化以及毛细管气相色谱的测定方法。运用石油醚-丙酮（P／P，2：1）混合溶剂提取，用氟罗里硅土进行层析净化，60ml石油醚／乙酸乙酯（V／V，9：1）进行洗脱，电子捕获-气相色谱测定，单点外标法定量。实验表明：土样中添加0．08mgkg^-1的氯氰菊酯、氰戊菊酯和溴氰菊酯3种农药混标时，方法回收率为89．67％～90．62％，添加0．40mgkg^-1时．方法回收率为91、07％～93．02％；操作中相对标准偏差（RSD）为2．02％～3．70％，最小检出量可达1．00pg。在检测色谱精密度实验中，5次测定3种农药混标，相对标准偏差（RSD）为1．37％～2．88％。实验表明，该法具有灵敏度高、操作简便、净化效果好、重现性好等特点。     

土壤中有机氯及拟除虫菊酯类农药的多残留分析技术

建立了以乙腈水溶液超声提取,弗罗里矽SPE柱净化,GC-ECD进行检测土壤中六六六、滴滴涕、氯氰菊酯、溴氰菊酯、六氯苯等29种有机氯和拟除虫菊酯类农药含量的方法,方法的加标回收率在70%～120%,检出限为0.0010～0.230mg·kg-1。方法适用于黑土、红土、壤土等不同类型土壤样品。     

拟除虫菊酯类农药的色谱分析法

拟除虫菊酯类杀虫剂具有用量低，效果好，杀虫谱广，对温血动物毒性低等优点，目前广泛用于防治农业害虫。在拟除虫菊酯的研究和生产过程中，在环境影响农药残留调查时都要求提供准确快速的测定方法。但是由于拟除虫菊酯分子结构的特点，它们都包含多个光学异构体，这些异体栖往往又具有不同的生物活性，因此必须解决异构物的分析方法问题，本总结了近年来拟除虫菊酯的气相和液相色谱分析方法进展，并介绍了作自己的工作经验。     

浓硫酸纯化-气相色谱法测定土壤中拟除虫菊酯农药残留

建立了土壤中拟除虫菊酯类农药新的前处理方法。样品以乙腈提取,浓硫酸-乙醇进行纯化,毛细管柱气相色谱法测定土壤中的拟除虫菊酯农药。结果表明:4种菊酯在3种土壤样品中的添加回收率在84.14%～105.51%之间,变异系数为1.24%～5.82%。该方法具有省时、省溶剂、操作简单、纯化效果好、实用性强的特点。     

拟除虫菊酯类农药微生物降解研究进展

拟除虫菊酯类农药是杀虫剂中的第三大类,这类农药残留已成为目前农产品中的主要农药残留类型之一。而微生物在降解农药残留中具有重要的作用,微生物降解技术已成为去除农药残留的绿色生产技术。拟除虫菊酯类农药的微生物降解国内外已有的研究主要集中在降解现象,菌株的分离、鉴定及生理生化特性,酶学,不同光学异构体的降解、降解途径等方面,本文对此进行了较详细的回顾,并对将来的研究方向进行了展望。     

土壤中拟除虫菊酯微生物降解研究

微生物降解是拟除虫菊酯类农药从土壤中消去的主要途径。本文介绍了拟除虫菊酯降解菌的分离鉴定、降解基因的克隆以及微生物降解机理研究的近期成果,综合介绍了拟除虫菊酯异构体选择降解的特征、原因以及可能产生的环境效应,重点分析了农药疏水性、土壤吸附、重金属、土壤养分及长期施肥、共存农药对土壤中拟除虫菊酯微生物降解的影响,最后对土壤微生物修复前景进行了展望。     

拟除虫菊酯类农药残留降解菌的筛选及其生理特性研究

从活性污泥的富集培养物中分离得到可降解几种拟除虫菊酯农药的菌株qw5,初步鉴定qw5为地衣芽孢杆菌 (Bacilliuslicheniformis)。菌株qw5在通气、pH7～ 8、温度 3 0℃左右的环境条件下生长较好。培养 5天 ,菌株qw5对氰戊菊酯、氯氰菊酯、溴氰菊酯的降解率分别为 5 3 .8%、41 .2 %和 61 .7%。经质谱分析 ,菌株qw5降解氰戊菊酯产生中间代谢产物 3 -苯氧基苯甲醛。qw5对小白鼠无致病力 ,对几种常用的抗生素敏感。盆钵和小区试验表明 ,菌株qw5对青菜中残留的拟除虫菊酯有明显去除效果。     

拟除虫菊酯类农药光降解的研究进展

拟除虫菊酯类农药的广泛使用,引起的环境问题及农业生产与日常生活中的安全问题日益突出。本文综述了拟除虫菊酯类农药的光降解行为,包括自然光照降解、紫外光照降解、光催化降解、光照下的微生物降解及辐照降解;探讨了影响光降解的因素,如光照强度、p H、氧气、溶剂、金属离子、腐殖质,及与其他农药的交互作用等。最后,总结了拟除虫菊酯类农药的光降解机理。     

超高效液相色谱-串联质谱法测定植物性农产品中24种拟除虫菊酯类农药残留

建立了植物性农产品中24种拟除虫菊酯类农药残留的超高效液相色谱-串联质谱快速检测方法。样品经QuEChERS前处理方法提取、净化、浓缩,选用电喷雾离子源（ESI）正离子模式测定,外标法定量。结果显示,24种拟除虫菊酯类农药在各自浓度范围内线性良好,相关系数（r）均在0.99以上,定量限在0.005～0.05 mg/kg。在0.01、 0.05、 0.10mg/kg 3个添加水平下,添加回收率在75.2%～114.0%,相对标准偏差为0.4%～10.9%。本方法检测稳定性好、基质影响小、检测时间短、检测结果准确,适用于日常检测工作中大批量植物性农产品的拟除虫菊酯类农药残留监测。     

气相色谱法对茶园土壤中3种农药残留量的检测

通过对来自六种不同茶园土壤的三种农药残留量的监测,对茶园环境质量现状进行了较系统的调查,并进行了茶园的污染评价。本研究以丙酮为提取剂,样品经提取和浓缩后,采用毛细管柱气相色谱分离,电子捕获检测器(ECD)检测农药残留,外标法定量。不同种类茶园土壤的农药残留量是不同的。用气相色谱法分析茶园土壤中农药残留,全面了解茶园中拟除虫菊酯类农药残留量现状,有利于更好地采取行之有效的措施降低农药残留量,对促进茶叶的出口贸易也起到重要的作用。     

土壤宏蛋白质组学之土壤蛋白质提取技术的发展

随着土壤宏基因组学的日益成熟和发展,作为后基因组时代重要技术平台的土壤宏蛋白质组学越来越受到关注。土壤宏蛋白质组学的研究是解析土壤宏基因功能的重要手段之一,对于碳氮磷的生物地球化学循环以及土壤有机质积累的研究具有重大价值,可将蛋白信息与相关的生态系统过程联系起来。但是,土壤蛋白含量少,样品复杂程度高,极大限制了土壤蛋白的分离提取和进一步分析。因此,通过改进和优化土壤蛋白的提取技术,得到高浓度的蛋白是土壤宏蛋白质组学研究的前提条件。本文总结了近几年来土壤蛋白提取方法,并对其适用的土壤性质以及适用的不同种类和功能的蛋白进行了分析。此外,本文也对现有的土壤蛋白提取技术以及土壤蛋白鉴定技术的方法改进进行了探讨。     

小麦田土壤中炔草酯GC-ECD检测方法研究及残留行为特征

采用乙腈振荡提取,GC-ECD测定,建立了小麦田土壤中炔草酯残留量的测定方法。在0.01~2.0 mg·kg-1质量浓度范围内,气相色谱峰面积与炔草酯质量浓度呈良好的线性关系,相关系数为R2=0.999 4。外标法定量,土壤中添加炔草酯质量分数分别为0.01、0.1 mg·kg-1和0.5 mg·kg-1,平均回收率分别为95.91%、89.50%和75.35%,相对标准偏差分别为2.66%、7.64%和4.23%,最低检出浓度为0.01mg·kg-1。检测结果表明,该测定方法前处理简便快速、成本低、结果准确,能够满足土壤中炔草酯残留量的分析要求。在山东和湖南开展的2年两地土壤田间试验结果表明,炔草酯在土壤中30 d的消解率均超过99%,理论半衰期为2.7~3.9d,属于易降解农药。     

Comparison of Chemical Extraction Methods for Determination of Soil Potassium in Different Soil Types

Determining potassium supply of soil plays an important role in intensive crop production, since it is the basis for balancing nutrients and issuing fertilizer recommendations for achieving high and stable yields within economic feasibility. The aim of this study was to compare the different extraction methods of soil potassium from arable horizon of different types of soils with ammonium lactate method (K_AL), which is frequently used as analytical method for determining the accessibility of nutrients and it is a common method used for issuing fertilizer recommendations in many Europe countries. In addition to the ammonium lactate method (K_AL, pH 3.75), potassium was extracted with ammonium acetate (K_AA, pH 7), ammonium acetate ethylenediaminetetraacetic acid (K_AAEDTA, pH 4.6), Bray (K_BRAY, pH 2.6) and with barium chloride (\(K_{BaCl_2 }\), pH 8.1). The analyzed soils were extremely heterogeneous with a wide range of determined values. Soil pH reaction \(\left( {pH_{H_2 O} } \right)\) ranged from 4.77 to 8.75, organic matter content ranged from 1.87 to 4.94% and clay content from 8.03 to 37.07%. In relation to K_AL method as the standard method, \(K_{BaCl_2 }\) method extracts 12.9% more on average of soil potassium, while in relation to standard method, on average K_AA extracts 5.3%, K_AAEDTA 10.3%, and K_BRAY 27.5% less of potassium. Comparison of analyzed extraction methods of potassium from the soil is of high precision, and most reliable comparison was K_AL method with K_AAEDTA, followed by a: K_AA, \(K_{BaCl_2 }\) and K_BRAY method. Extremely significant statistical correlation between different extractive methods for determining potassium in the soil indicates that any of the methods can be used to accurately predict the concentration of potassium in the soil, and that carried out research can be used to create prediction model for concentration of potassium based on different methods of extraction.     

Evaluation of Extraction Methods for Plant-Available Soil Cadmium to Wheat by Several Extraction Methods in Cadmium-Polluted Paddy Field

To develop a new method for the extraction of plant-available cadmium (Cd), the correlation between the Cd content of polluted soil extracted with several extractants and the Cd content of wheat plants (variety “A” Triticum aestivum L.) was examined. Among the HCI concentrations of soil extractants tested, the content of 0.025 mol L^?1 HCI (HCl_0.025)-extractable Cd of soil showed a significant correlation with the Cd content of wheat grain and Cd uptake by shoot. The correlation between the soil Cd content extracted with 1 mol L^?1 NH₄Cl and the Cd content of wheat grain was nearly the same as that in the case of HCI_0.025. In contrast, other reagents such as MgCl₂, diethylenetriaminepentaacetate (DTPA) and tetra-sodium pyrophosphate (Na₄P₂O₇) could not give a good correlation between the extractable Cd content of soil and the Cd content of wheat grain. Therefore, it was considered that HCl_0.025-extractable Cd is a suitable indicator of the content of plant-available Cd of soil to wheat. This extraction method can be applied to weakly acid Grey Lowland soil. Using the equation for the relation between the content of HCl_0.025-extractable Cd of soil and the Cd content of grain of the wheat variety “A”, the Cd content of grain of other 11 wheat varieties was evaluated. The wheat variety “A” showed the lowest absorption of Cd. The Cd content of variety “B” grain was located on the regression line of that of variety “A”, suggesting that both varieties exhibited the lowest ability to absorb Cd among the varieties tested. Grain yields of both “A” and “B” varieties were reasonably high. On the other hand, other varieties showed a substantially high ability to absorb soil Cd compared with the varieties “A” and “B”. The new method proposed for the determination of the content of plantavailable Cd proved to be suitable for the evaluation of plant-available Cd of soil and also for the screening of wheat varieties with a high or low Cd accumulation capacity in grain.     

三种土壤微生物总DNA提取方法的比较

本文对3种常用的土壤微生物总DNA提取方法Martin法、高盐改进法及试剂盒法进行了比较,并通过DNA得率、纯度及16S rDNA V3可变区的PCR扩增结合DGGE法（denatumg gradient gel electrophoresis）,分别对3种方法进行评价。结果表明,3种方法提取的DNA均能满足土壤微生物多样性分析的要求。其中试剂盒方法操作简单,提取的DNA质量较高,但DNA得率较低且成本昂贵。Martin法和高盐改进法用时较长,DNA得率较高,纯度较低,但对后续PCR扩增和DGGE分析没有明显影响,且成本低廉。     

茶园土壤微生物总DNA不同提取方法的比较

传统的微生物分离培养方法,在反映茶园土壤微生物基因信息上有很大的局限性,因此,目前逐步被分子生态学的方法替代,而获得高质量、大片段、无偏好的土壤微生物总DNA则是茶园土壤微生物分子生态学研究的基础。本文采用SDS高盐法、变性剂加SDS高盐法、脱腐SDS高盐法、CTAB法和Krsek改进法5种土壤微生物DNA提取方法分别从茶园土壤微生物中提取总DNA,并对5种方法提取的DNA的片段大小、质量和产量进行了综合评价。结果表明,Krsek改进法提取到的DNA片段最大（〉23kb）、纯度最高（OD2UOD280〉1．70;OD2UOD230〉1．35）、产量较高（〉34．50μg／gdrysoil）且不需纯化就可以用于PCR扩增和RFLP分析。因此,Krsek改进法是一种高效、可靠且适合于茶园土壤微生物分子生态学研究的DNA提取方法。     

渭北旱塬小麦不同栽培模式对土壤硝态氮残留的影响

在陕西渭北旱塬进行了4年田间小麦试验,研究了旱地不同栽培模式、施氮量和种植密度对土壤硝态氮残留累积的影响。结果表明,种植小麦4年后,0-200 cm土壤剖面中残留硝态氮为29.87~462.59 kg/hm2,且主要积累在80-160 cm土层,土壤氮库不仅明显,且残留比前3年土壤剖面显著下移(前3年主要累积在100 cm),差异达显著和极显著水平;不同栽培模式和种植密度0-200 cm土层硝态氮残留累积规律及其小麦籽粒吸氮量基本相似,排序均为:地膜覆盖>常规种植>秸秆覆盖>垄沟种植;随施氮量的增加土壤硝态氮残留量也相应增加,N0处理0-200 cm土壤平均硝态氮残留量为57.69 kg/hm2,N120处理平均为97.04 kg/hm2,虽然高于无氮处理,但两者差异未达到显著水平,N240处理平均为355.43 kg/hm2,比前者增加的幅度更大,其差异达到极显著水平。因施氮肥而增加的土壤硝态氮残留量为14.9~401.18 kg/hm2,平均占4年施氮量的19.59%,其中地膜覆盖占26.07%,常规种植占20.98%,秸秆覆盖占17.46%,垄沟种植种植占13.87%。     

Characterization of Soil Phosphorus in Differently Managed Clay Soil by Chemical Extraction Methods and 31P NMR Spectroscopy

Changes in land use alter the natural cycling of phosphorus (P) in soil. Understanding the chemical nature of these changes is important when developing sustainable management practices for cultivated soils. In this study, we evaluated the ability of commonly used laboratory methods to characterize land use–induced changes in various P pools. Also, the characteristics of soil P revealed by different methods are discussed. Soil samples were taken from three differently managed field plots of the same clay soil: uncultivated grassland and organic and conventional crop rotations. Soil P reserves were characterized using Chang and Jackson and Hedley sequential fractionation procedures and by sodium hydroxide (NaOH)–ethylenediaminetetraacetic acid (EDTA) extraction followed by ³¹P NMR spectroscopy. Both of the tested fractionation methods identified differences in the P pools and provided evidence regarding land use–induced changes. However, the ³¹P NMR analysis suggests that the quality of organic P in this soil was not affected by the change in land use.     

土壤微生物总DNA提取方法的比较

采用4种土壤DNA提取方法提取了5种类型土壤的微生物总DNA，并对4种提取方法的DNA提取效果进行综合分析，进一步通过PCR—DGGE扩增提取DNA中的细菌16S rDNA片段，并对扩增产物进行DGGE电泳分析。结果表明，SDS-高盐缓冲液法抽提的DNA得率最高，SDS-酚氯仿抽提法的DNA得率最低。DNA的纯度，以BIO-101 DNA Extraction Kit试剂盒法最高，改进试剂盒法纯度最低。通过PCR-DGGE分析土壤微生物多样性结果表明，BIO-101 DNA Extraction Kit试剂盒法提取的DNA代表的微生物多样性最全，而SDS酚氯仿法抽提的DNA代表性最差。