衍生-气相色谱法测定水产品中的游离甲醛

建立了水产品中游离甲醛残留量的衍生-气相色谱快速检测方法,对衍生剂、抗干扰剂、萃取剂、色谱条件进行了研究.用HP-5 (30 m×0.32 mm i.d.,0.25 μm)毛细管色谱柱,程序升温,γ-ECD检测器,外标法定量.甲醛的检出限为0.05 mg/kg,在0.1～20.0 mg/L范围内,其线性相关系数R2=0.9994,标准偏差为0.041,在0.5、 1.5、 5.0 mg/kg 3个添加水平下回收率为89.6%～102.6%.3个实验室间的RSD为2.7%～4.4%.     

盐酸提取-液相色谱-原子荧光联用技术检测水产品中甲基汞等汞化合物

建立了HCl提取,高效液相色谱与原子荧光联用技术测定水产中无机汞、甲基汞、乙基汞形态的分析方法。对前处理方法和液相色谱的最佳参数进行优化,实验表明,3种汞化合物的线性范围为0~100μg/L,相关系数(r)均优于0.9990,检出限在0.3~0.6μg/L之间,汞化合物各形态的RSD均小于5%,加标回收率在78.8%~116.8%之间,标准物质(GBW10029),(GBW09101B)中汞形态的测定值均在标准值范围内,参加甲基汞FAPAS国际比对,测定结果的Z比分数为1.0,故本方法适用于水产品中汞化合物形态的分析测定。     

Speciation analysis of mercury in sediments, zoobenthos and river water samples by high-performance liquid chromatography hyphenated to atomic fluorescence spectrometry following preconcentration by solid phase extraction

A high-pressure microwave digestion was applied for microwave-assisted extraction (MAE) of mercury species from sediments and zoobenthos samples. A mixture containing 3 mol L⁻¹ HCl, 50% aqueous methanol and 0.2 mol L⁻¹ citric acid (for masking co-extracted Fe³⁺) was selected as the most suitable extraction agent. The efficiency of proposed extraction method was better than 95% with R.S.D. below 6%. A preconcentration method utilizing a “homemade” C18 solid phase extraction (SPE) microcolumns was developed to enhance sensitivity of the mercury species determination using on-column complex formation of mercury-2-mercaptophenol complexes. Methanol was chosen for counter-current elution of the retained mercury complexes achieving a preconcentration factor as much as 1000. The preconcentration method was applied for the speciation analysis of mercury in river water samples. The high-performance liquid chromatography-cold vapour atomic fluorescence spectrometric (HPLC/CV-AFS) method was used for the speciation analysis of mercury. The complete separation of four mercury species was achieved by an isocratic elution of aqueous methanol (65%/35%) on a Zorbax SB-C18 column (4.6 mm × 150 mm, 5 μm) using the same complexation reagent (2-mercaptophenol). The limits of detection were 4.3 μg L⁻¹ for methylmercury (MeHg⁺), 1.4 μg L⁻¹ for ethylmercury (EtHg⁺), 0.8 μg L⁻¹ for inorganic mercury (Hg²⁺), 0.8 μg L⁻¹ for phenylmercury (PhHg⁺).     

快速高效液相色谱-串联质谱法同时测定水产品中5类33种药物残留

建立了快速高效液相色谱-串联质谱法(RRLC-MS/MS)同时测定水产品中四环素类、喹诺酮类、磺胺类、磺胺增效剂和三苯甲烷类共5大类33种药物残留的方法。样品用Na2EDTA-Mcllvaine缓冲溶液及乙腈提取,正己烷脱脂后,用RRLC进行分离。在电喷雾正离子模式下,以动态多反应监测(Dynamic MRM)方式采集数据进行定性与定量分析。33种药物在相应的浓度范围内线性良好,相关系数均大于0.99;在3个不同浓度添加水平下,平均回收率为63.6%～115.2%;相对标准偏差(RSD)为4.6%～14.6%;检出限(LOD,S/N=3)和定量限(LOQ,S/N=10)分别为0.1～2.0μg/kg和0.5～5.0μg/kg。本方法简便快速、灵敏可靠,适用于水产品中药物多残留的同时快速定性与定量测定。     

液相色谱-串联质谱法测定水产品中麻醉剂MS-222残留

建立了液相色谱-串联质谱法测定水产品中麻醉剂3-氨基苯甲酸乙酯甲基磺酸盐(MS-222)残留量的方法。提取液为50%的甲醇及乙酸-乙酸钠缓冲溶液,提取液经C18固相萃取柱净化处理后用液相色谱-串联质谱仪进行测定,外标法定量。流动相为0.5%的甲酸溶液和乙腈(V:V=60:40),流速为0.2 mL/min。该方法的线性范围为0.001～1.0 mg/L,相关系数大于0.999,检出限为1μg/kg,定量限为2μg/kg。加标回收率可以达到80%～110%。     

固相萃取-高效液相色谱/串联质谱法测定水产品中硫酸新霉素残留量

建立了一种分析水产品中硫酸新霉素残留量的固相萃取-高效液相色谱/串联质谱法。样品经三氯乙酸水溶液提取,固相萃取小柱净化。用带加热电喷雾离子源的高效液相色谱/串联质谱以选择反应离子监测(SRM)正离子模式检测,基质标准曲线定量。结果显示,在草鱼、斑点叉尾鮰、鳗鲡、南美白对虾和甲鱼空白肌肉中添加硫酸新霉素水平为25~1 000μg/kg时,其加标回收率为91.04%~114.57%,相对标准偏差为1.91%~9.62%。硫酸新霉素的检测限为10μg/kg,定量限为25μg/kg。方法适用于水产品中硫酸新霉素残留量的测定,也适用于硫酸新霉素在水产动物体内组织分布和消除研究。     

淹水区生态型护坡设计及抗冻融性能分析

针对淹水区坡面进行护坡的必要性和传统护坡技法的缺陷,提出了应用生态型护坡技法——中日植生材料（一种新型生态植生材料）、生态混凝土（多孔、透水性混凝土）、卵石（自然石）等近自然界材料的组合,进行设计、护坡．国家863专项“镇江水环境处理”中的生态堤采用生态型护坡技法进行设计,通过对该技法中组成材料的分析和生态混凝土耐久性的主要影响因素——冻融进行调查、研究,认为所提出的生态护坡技法不仅能充分保证护坡工程安全性、经济性,还可维持和改善生态环境,谋求与生态系统的调和或共生,创造舒适的环境,而且所用生态混凝土具有良好的抗冻融性．     

黄土高原植被恢复前景及策略研究进展

对黄土高原地区森林植被恢复前景及策略研究进展进行了概述和分析。分别从黄土高原地区森林植被恢复前景、植被恢复总体思路、植被生态建设分区这3个方面的相关研究情况进行了综述。同时,围绕“黄土高原尤其是厚层黄土塬区是否有可能恢复森林植被”这一焦点问题展开论述,针对几种不同的观点进行了分析和讨论,同时,针对这一问题提出了几点看法。     

条件植被温度指数干旱监测方法的研究与应用

综合应用归一化植被指数(NDVI)和土地表面温度(LST),提出了条件植被温度指数(VTCI)的概念,并将其用于干旱监测。VTCI的定义既考虑了区域内NDVI的变化,又强调了NDVI值相等时LST的变化,可解释为NDVI值相等时LST差异的比率。分别以陕西关中平原地区和美国大平原南部地区为研究区域,应用AVHRR和MODIS卫星遥感反演的NDVI和LST产品,以及累计降水量和降水偏差数据,证实了条件植被温度指数是一种近实时的干旱监测方法。     

Global vegetation change analysis based on MODIS data in recent twelve years①

Vegetation cover change is critical for understanding impacts and responses of vegetation to climate change. A study found that vegetation in the regions between 45°N-70°N was increasing using normalized difference vegetation index( NDVI) from 1981 to 1991 ten years ago. The global vegetation growth has changed because of climate change in recent twelve years( 2001- 2012). After thorough analysis based on satellite data,it is found that it is evident that the global vegetation changed( NDVI) little,and it is increasing slightly in Northern hemisphere while it is decreasing slightly in Southern Hemisphere. For different latitudes,vegetation is increasing 0.17% every year from 60°N to 70 °N( R~2= 0.47,P 0.013),while the vegetation is decreasing 0.11% every year from 10°N to 10° S( R~2= 0.54,P 0.004). For different continents,the vegetation in South America is decreasing 0.16% every year( R~2= 0.78,P 0.0001) and it is increasing 0.05% every year in Asia( R~2= 0.28,P 0.072) and 0.25% every year in Oceania( R~2= 0.24,P 0.1). The analysis of global vegetation in different seasons indicates that spatial distribution of global temperature and water vapor will affect the spatial distribution of vegetation,in turn,the spatial distribution of vegetation will also regulate the global temperature and water vapor spatial distribution at large scale. The growth and distribution of vegetation are mainly caused by the orbit of the celestial bodies,and a big data model based on gravitational-magmatic change with the solar or the galactic system as its center is proposed to be built for analyzing how the earth's orbit position in the solar and galaxy system affects spatial-temporal variations of global vegetation and temperature at large scale. These findings promise a holistic understanding of the global climate change and potential underlying mechanisms.