不同反胶束体系萃取纤维素酶的条件优化对比研究

采用3种不同的表面活性剂双(2-乙基己基)磺基琥珀酸钠AOT、十六烷基三甲基溴化铵CTAB及鼠李糖脂RL)溶于正己醇/异辛烷相构建不同的反胶束体系,并对比研究了不同反胶束体系萃取纤维素酶的优化条件.分别探讨了水相pH值、表面活性剂浓度、离子强度和离子种类对纤维素酶萃取效率的影响.实验结果如下:在实验条件下,AOT、CTAB和RL 3种反胶束体系水相最佳pH值分别为3.0、8.0和3.0;表面活性剂最佳浓度依次为:AOT 23.7mmol/L、CTAB 15mmol/L和RL 2.75mmol/L;水相中NaCl浓度会影响纤维素酶的萃取率,3种表面活性剂构建的反胶束体系萃取纤维素酶的萃取率均随着盐离子浓度的增大而降低;水相中离子种类也会影响纤维素酶的萃取率.比较不同反胶束体系在最佳条件下萃取纤维素酶的最佳萃取率:CTAB>AOT>RL.     

密度分离法提取土壤中微塑料的优化

为探究一种简单、经济和可靠的微塑料分离提取手段,设立了11种(F1~F11)具有不同体积比的饱和NaCl和饱和NaI溶液的混合溶液,将混合液作为浮选液来提取土壤中的4种类型(聚乙烯,PE;聚苯乙烯,PS;聚氯乙烯,PVC;聚对苯二甲酸乙二醇酯,PET)微塑料,同时对浮选过程进行了改进.结果表明:当单独使用NaCl溶液浮选时,微塑料的总提取率为55.83%,但随着NaI所占体积比的不断增加,微塑料的总提取率基本呈上升趋势,在NaCl:NaI=1:1时总提取率超过了90%,在只有NaI的条件下总提取率高达96.67%;在F1~F11的任意条件下,PE和PS表现为较高的提取率,均超过了86.67%;PVC和PET在单独使用NaCl溶液浮选时提取率极低,在NaCl:NaI=1:1条件下提取率分别为93.33%和90%,接近单独使用NaI溶液浮选时的提取率;F1~F11任意条件下,低密度微塑料PE和PS的提取率之和均高于高密度微塑料PVC和PET的提取率之和,但在F6~F11条件下提取率差值不大.根据提取结果并结合经济成本等多方面因素考虑,建议使用NaCl:NaI=1:1的混合溶液来分离土壤中的微塑料.     

三种模拟消化液对土壤重金属的提取性比较

为了解不同方法的模拟消化液对土壤重金属提取性的差异性,比较了国际上广泛使用的3种代表性体外消化方法的模拟消化液(SBET, Simple Bioaccessibility Extraction Test;PBET, Physiologically-Based Extraction Test;SGET, Simple Gastrointestinal Extraction Test)对土壤中Cu、Zn、Pb和Cd的溶解效果.结果表明,3种方法的模拟消化液对土壤重金属的提取效果存在显著的差异.其中,3种模拟消化液对土壤中Zn和Cd的提取能力顺序为SBET>PBET>SGET;当胃液消化物进入肠液后,土壤中Zn、Cd和Pb在PBET及SGET中的溶解度都显著降低,而对于Cu,由于消化酶(胃蛋白酶、胰液素和胆汁盐)的络合作用,其在肠液中的溶解度不一定低于相应的胃液,因此土壤中Zn、Pb和Cd在胃液中的溶解度代表其在消化道中能被吸收的最大值,即其有可能被人体吸收的最大量.所以出于预防和保护的目的,在土壤重金属污染健康风险评价中可用只含有胃液的模拟消化液(如SBET法)评估土壤Zn、Cd和Pb的生物可接受性,但胃液中的提取量并不一定能代表土壤Cu在消化道中能被吸收的最大值,建议使用由胃液和肠液组成,且添加了相应消化酶的模拟消化液(如PBET法)对其生物可接受性进行评估.     

微囊藻毒素的提取和提纯研究

对采自云南滇池水华蓝藻细胞中的微囊藻毒素 (Microcystins,MCs)的提取与提纯方法进行了研究 .结果表明 ,在藻细胞干重浓度为 2 0g·L-1下 ,与不同甲醇浓度提取液相比 ,4 0 %甲醇溶液可以最有效地从藻细胞中提取出MC RR和MC LR .将MCs提取液过Waters固相萃取小柱后 ,用 70 %甲醇溶液洗脱吸附于柱上的MCs ,可以分别获得 7 3%和 3 5 %纯度的MC RR和MC LR .通过观察洗脱液的颜色变化 ,收集蓝绿色和橘黄色后面流出的基本无色的洗脱液 ,可以获得纯度为 2 8 6 %和12 9%的MC RR和MC LR .     

Selective extraction and separation of Fe, Mn oxides and organic materials in river surficial sediments

In order to investigate the adsorption mechanism of trace metals to surficial sediments （SSs）, a selective extraction procedure was improved in the present work. The selective extraction procedure has been proved to selectively remove and separate Fe, Mn oxides and organic materials （OMs） in the non-residual fraction from the SSs collected in Songhua River, China. After screening different kinds of conventional extractants of Fe and Mn oxides and OMs used for separation of heavy metals in the soils and sediments, NH2OH .HCl （0.1 mol/L） ＋ HNO3 （0.1 mol/L）, （NH4）2C2O4 （0.2 mol/L） ＋ H2C2O4 （pH 3.0）, and 30% of H2O2 were respectively applied to selectively extract Mn oxides, Fe/Mn oxides and OMs. After the extraction treatments, the target components were removed with extraction efficiencies between 86.09%--3.36% for the hydroxylamine hydrochloride treatment, 80.63%- 101.09% for the oxalate solution extraction, and 94.76%-102.83% for the hydrogen peroxide digestion, respectively. The results indicate that this selective extraction technology was effective for the extraction and separation ofFe, Mn oxides and OMs in the SSs, and important for further mechanism study of trace metal adsorption onto SSs.     

活性污泥中一氧化氮还原酶的提取和测定优化

通过正交实验,研究了超声破碎法和低温高压破碎法提取一氧化氮还原酶（nitric oxide reductase,nor）的活性,分析了超声强度和次数,破碎压力和次数,裂解液的添加量等因素对于胞内可溶性蛋白和核酸（DNA）的释放与提取nor活性的影响.根据活性污泥中酶的催化特性以及其他实验条件,完善了nor催化活性的测定方法.结果表明超声法提取nor的参数应设定为,超声次数为100次,超声强度为500W,裂解液的添加量为0.1mL.低温高压破碎法提取nor的参数应设定为破碎次数为4次,破碎压力为50MPa,裂解液的添加量为0.1mL.低温高压破碎法下的胞内可溶性蛋白和DNA的释放量与nor的最大催化活性要高于超声破碎法.此外,在nor催化活性的测定方法中,nor活性测定终点时间应为15min.     

硝化污泥胞外聚合物分层组分提取方法的比较

采用温和加热法、超声法、超声+振荡法和离心法4种方法提取硝化污泥松散结合型胞外聚合物(LB-EPS),及乙二胺四乙酸(EDTA)法、甲醛+NaOH法、甲醛+超声、阳离子树脂法(CER)和加热法提取硝化污泥紧密结合型胞外聚合物(TB-EPS),通过化学分析结合三维荧光(3DEEM)光谱对各提取方法进行比较.结果表明,LB-EPS和TB-EPS的最优提取方法分别为温和加热法和甲醛+Na OH法,TOC提取量分别为16.82、58.43 mg·g~(-1).三维荧光光谱显示温和加热法能有效提取LB-EPS中的类色氨酸和类腐殖酸;甲醛+NaOH法、CER和加热法提取的TBEPS中物质最为全面,主要包括类色氨酸、类腐殖酸和类酪氨酸.TB-EPS三维荧光浓度效应分析表明荧光峰位置与EPS浓度变化无关;类腐殖酸和类酪氨酸荧光峰强度随EPS浓度降低而减小,分别呈二项式和对数关系.     

土壤气相抽提过程中多孔介质扰动的数值分析

基于质量守恒与流体达西定律推导水气二相流动的连续性微分方程,进而结合饱和度~相对渗透率~毛细压力耦合关系构建二相流动数学模型,并建立多孔介质孔隙度变化与水气二相饱和度之间的数学关系,最终实现多孔介质扰动时空变化的定量表征.案例模拟分析结果表明:对于特定场地而言,抽提影响带的空间形态与抽提真空度密切相关,抽提真空度越大,影响半径及影响带内的气流速度越大,本案例中抽提真空度在11kPa和31kPa时的抽提影响半径分别达到8.5m和9m;在抽提过程中,孔隙度及渗透率随时间呈现先增加后稳定的显著变化,达到稳定所需的时长及其变幅则与离抽提段的空间距离成反相关,抽提压力为0.7′105Pa、特征参数 =0.8的情景模拟显示:距离抽提段1m的P1点在约40min后孔隙度达到稳定、增幅为0.0387,而较远的P4点,距抽提段水平距离为3m,约在60min后达到稳定、增幅为0.0031,相应地,P1和P4点介质渗透率分别从1.18×10-11m2增加至2.22×10-11与1.25×10-11m2;在相同抽提压力下,孔隙度增幅与关键参数 值成正相关,抽提压力为0.9×105Pa、 =0.1和0.8时的孔隙度最大增幅分别约为0.009和0.055;相同参数 条件下,孔隙度增幅与抽提压力成正相关, =0.8、抽提压力为0.7×105Pa时的孔隙度最大增幅则达到0.066.     

超声辅助分散液液微萃取-气相色谱检测污泥中氯苯

采用超声辅助分散液液微萃取结合气相色谱(UAE-DLLME-GC-ECD)检测了污泥中6种氯苯化合物.用丙酮作为萃取污泥样品中氯苯的萃取剂,通过改变萃取剂类型和用量、超声时间以及离子强度等影响因子的实验,确定了最优条件的关键性控制参数.结果表明,6种氯苯的相关系数r2=0.9993~0.9999,相对标准偏差RSD=3.2%~4.4%,检测限LOD为0.001~0.2μg/kg,对造纸、印染和市政3种污泥样品检测的回收率分别为89.2%~103.8%, 94.5%~112.1%和89.1%~104.3%.该方法检测污泥中的氯苯不仅具有快速、灵敏和重复性好的特点,而且相对于传统方法,可以节省大量对人体有毒害作用的有机溶剂和分析时间.     

好氧/厌氧污泥胞外聚合物(EPS)的提取方法研究

采用5种方法对同一污泥在好氧和厌氧条件下的胞外聚合物(EPS)进行了提取试验研究.结果表明,甲醛-NaOH和H2SO4法对EPS的提取产量最高,分别为232·0mg·g~(-1)和159·7mg·g~(-1),且无大量细胞自溶发生,是比较有效的提取方法;与对照方法相比较,阳离子交换树脂(CER)和戊二醛提取法却存在严重缺陷.两种氧环境条件下污泥EPS中蛋白质的含量均最高,占EPS总量的50%~80%;其次为胞外多糖和DNA.污泥在经由好氧环境到厌氧环境的转变过程中,EPS中主要成分蛋白质和DNA含量降低较为明显,其厌氧/好氧状态下的相应含量比值为0·59~0·91.试验中也发现,提取步骤和检测手段对结果的影响最大.     

Tenax提取预测老化土壤中多环芳烃的生物有效性

利用聚2,6-二苯基对苯醚(poly(2,6-diphenyl-p-phenylene oxide),商品名Tenax-TA)提取来自9个老化农田土壤中的多环芳烃(PAHs),并应用Tenax-TA评价老化土壤中PAHs对赤子爱胜蚓(Eisenia Fetida)的生物有效性.结果表明,多年老化土壤中污染物的主要组成为4环以上的PAHs;蚯蚓较易富集低环PAHs,对高环PAHs富集能力较差;400h Tenax连续提取实验得出快速、慢速和极慢速吸附速率常数数量级分别为:10-1~10-2、10-2~10-3、10-4~10-6;而快速、慢速和极慢速解吸比率分别为0.02~0.27、0.01~0.33和0.40~0.95.Tenax 6h单点提取PAHs的量与蚯蚓体内PAHs富集量显著相关,表明6h Tenax对多年老化土壤中PAHs的提取量可以用来作为其生物有效性的评价方法.     

Cloud point extraction coupled with HPLC-UV for the determination of phthalate esters in environmental water samples

A method based on cloud point extraction was developed to determine phthalate esters including di-ethyl-phthalate （DEP）, di- （2-ethylhexyl）-phthalate （DEHP） and di-cyclohexyl-phthalate （DCP） in environmental water samples using high-performance liquid chromatography separation and ultraviolet detection （HPLC-UV）. The non-ionic surfactant Triton X-114 was chosen as extraction solvent. The parameters affecting extraction efficiency, such as concentrations of Triton X-114 and Na2SO4, equilibration temperature, equilibration time and centrifugation time were evaluated and optimized. Under the optimum conditions, the method can achieve preconcentration factors of 35, 88, 111 and detection of limits of 2.0, 3.8, 1.0 ng/ml for DEP, DEHP and DCP in 10-ml water sample, respectively. The proposed method was successfully applied to the determination of trace amount of phathalate esters in effluent water of the wastewater treatment plant and the lixivium of plastic fragments.     

超声波提取在近海沉积物油类测定中的应用

根据紫外分光光度法测定近海沉积物油类实践,探讨了超声波提取技术在近海沉积物油类测定中的应用。试验结果表明,应用超声波提取技术进行近海沉积物油类样品的前处理,时间短(8min),提取效率高(达95％以上),有机溶剂用量小(约25.0mL),操作简便易行,仅需2次提取,工作曲线线性好(r=0．999);对实际样品的分析测试,其相对标准偏差小于2．0％,回收率可达95．0％以上,结果准确可靠;与经典的索氏提取法相比,结果无显著差异。     

Determination of volatile organic compounds in river water by solid phase extraction and gas chromatography

A simple, rapid, and reproducible method is described employing solid-phase extraction (SPE) using dichloromethane followed by gas chromatography (GC) with flame ionization detection (FID) for determination of volatile organic compound(VOC) from the Buriganga River water of Bangladesh. The method was applied to detect the benzene, toluene, ethylbenzene, xylene and cumene(BTEXC) in the sample collected from the surface or 15cm depth of water. Two-hundred ml of n-hexane-pretreated and filtered water samples were applied directly to a C18 SPE column. BTEXC were extracted with dichloromethane and average concentrations were obtained as 0. 104 to 0.372 μg/ml. The highest concentration of benzene was found as 0.372 μg/ml with a relative standard deviation (RSD) of 6.2%, and cumene was not detected. Factors influencing SPE e.g., adsorbent types, sample load volume, eluting solvent, headspace and temperatures, were investigated. A cartridge containing a C18 adsorbent and using dichloromethane gave better performance for extraction of BTEXC from water. Average recoveries exceedina 90% could be achieved for cumene at 4℃ with a 2.7% RSD.     

三种土壤中土霉素浸提方法的比较研究

以棕壤、褐土和红壤为研究对象,比较了不同浸提方法,不同浸提剂对土壤中土霉素的浸提效率.结果表明,在所用的3种方法中,采用振荡浸提方法,以及Na2EDTA-McIlvaine缓冲液对土霉素具有稳定、高效的浸提回收率.土霉素形态初步分析连续浸提步骤为:以H2O、0.1mol/L CaCl2、和Na2EDTA-McIlvaine缓冲液为浸提剂依次浸提可分别得到水溶态、可交换态、吸附态和固定态土霉素.3种土壤中土霉素形态呈现吸附态>可交换态>水溶态的规律.     

用萃取剂LIX84I从电子废弃物处理液中选择性萃取铜

考察了相比、水相pH、混合时间等因素对LIX84I萃取铜的影响，结果表明：这些因素对铜的萃取率都有一定的影响，最优化的条件是有机相为30％LIX84I＋70％煤油、室温、相比=2：1、出口水相pH值=2．0、搅拌速度=910r／min、萃取级数为3级，每级的时间为3min。对铜进行三级萃取和一级反萃，可以得到符合电积要求的硫酸铜溶液，萃取率和反萃取率分别可以达到94．6％和97．8％。     

基于无人机可见光影像的绿色植被提取

在分析健康绿色植被光谱特性及无人机可见光影像典型地物各波段像元值差异的基础上,提出一种综合利用红、绿、蓝3个可见光波段信息的新型绿色植被指数——差异增强植被指数（DEVI）.利用该指数及其他8种常见可见光植被指数结合不同阈值方法提取研究区域绿色植被信息,并采用地表真实感兴趣区和基于SVM的监督分类方法进行精度量化评价.结果表明：由DEVI计算的植被指数灰度影像直方图具有良好双峰形态,可利用双峰直方图阈值法快速确定阈值,且阈值一般位于0.9~1之间;同时,DEVI提取精度明显优于其余8种植被指数,且采用双峰直方图阈值法时,总体精度为98.98%,Kappa系数为0.9791,相对误差为1/83.为验证DEVI是否具有良好的可适用性及可靠性,选取3种典型植被覆盖区域进行可行性验证,结果表明：利用DEVI可高精度提取建筑密集区域和植被零散分布区域的绿色植被信息,总体精度分别为98.42%和98.56%,Kappa系数分别为0.9610和0.9635,相对误差分别为1/125和1/91;而植被集中分布区域提取精度略低于上述2种典型区域,总体精度为97.40%,Kappa系数为0.9371,相对误差为1/53.因此,提出的差异增强植被指数——DEVI可以有效、高精度、低成本提取不同植被覆盖典型区域无人机可见光影像中的绿色植被信息,为陆地生态系统中的绿色植被监测研究提供一种可行性方法.     

TiO2 nanotubes as solid-phase extraction adsorbent for the determination of polycyclic aromatic hydrocarbons in environmental water samples

An analytical method based on TiO2 nanotubes solid-phase extraction (SPE) combined with gas chromatography (GC) was established for the analysis of seven polycyclic aromatic hydrocarbons (PAHs): acenaphtylene, acenaphthene, anthracene, fluorene, phenanthrene, fluoranthene and pyrene. Factors a ecting the extraction e ciency including the eluent type and its volume, adsorbent amount, sample volume, sample pH and sample flow rate were optimized. The characteristic data of analytical performance were determined to investigate the sensitivity and precision of the method. Under the optimized extraction conditions, the method showed good linearity in the range of 0.01–0.8 g/mL, repeatability of the extraction (RSD were between 6.7% and 13.5%, n = 5) and satisfactory detection limits (0.017–0.059 ng/mL). The developed method was successfully applied to the analysis of surface water (tap, river and dam) samples. The recoveries of PAHs spiked in environmental water samples ranged from 90% to 100%. All the results indicated the potential application of titanate nanotubes as solid-phase extraction adsorbents to pre-treat water samples.     

新型吸附搅拌棒被动采样器研制及应用——基于多壁碳纳米管的改性

结合传统被动采样器原理和新发展的吸附搅拌棒技术,研制了以多壁碳纳米管-聚二甲基硅氧烷(MWCTNs/PDMS)作为涂层的新型吸附搅拌棒被动采样器,并以苯酚(PhOH)、己烯雌酚(DES)和铅(Pb)作为目标污染物,考察被动采样器其吸附性能,优化其吸附条件.结果表明,与商业化PDMS涂层吸附搅拌棒被动采样器相比,含MWCTNs/PDMS涂层吸附搅拌棒被动采样器能更快达到吸附平衡时间、具有更大的饱和吸附容量.甲醇是PhOH和DES优良解吸剂,0.6mol/L HNO₃为Pb最优解吸剂.该新型被动采样器重复使用50次以上其解吸效率仍能达到70%以上,具有良好的稳定性和重复利用效果.     

Efficient removal of naphthalene-2-ol from aqueous solutions by solvent extraction

Naphthalene-2-ol is a typical biologically recalcitrant pollutant in dye wastewater.Solvent extraction of naphthalene-2-ol from aqueous solutions using mixed solvents was investigated.Various extractants and diluents were evaluated,and the effects of volume ratio of extractant to diluent,initial p H,initial concentration of naphthalene-2-ol in aqueous solution,extraction time,temperature,volume ratio of organic phase to aqueous phase(O/A),stirring rate and extraction stages,on extraction efficiency were examined separately.Regeneration and reuse of the spent extractant were also investigated.Results showed that tributyl phosphate(TBP) achieved 98% extraction efficiency for naphthalene-2-ol in a single stage extraction,the highest among the 12 extractants evaluated.Extraction efficiency was optimized when cyclohexane and n-octane were used as diluents.The solvent combination of 20% TBP,20% n-octanol and 60% cyclohexane(V/V) obtained the maximum extraction efficiency for naphthalene-2-ol,99.3%,within 20 min using three cross-current extraction stages under the following extraction conditions:O/A ratio of 1:1,initial p H of 3,25°C and stirring rate of 150 r/min.Recovery of mixed solvents was achieved by using 15%(W/W) Na OH solution at an O:A ratio of 1:1 and a contact time of 15 min.The mixed solvents achieved an extraction capacity for naphthalene-2-ol stably higher than90% during five cycles after regeneration.