通过式固相萃取/超高效液相色谱-串联质谱法测定蔬菜中18种农药残留

建立了超高效液相色谱-串联质谱(UPLC-MS;MS)快速测定蔬菜中18种农药残留的方法.样品经乙腈提取后,经Oasis PRiME HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3 C18(50 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析.结果表明,18种农药在0.5—50μg·L^-1范围内线性关系良好(r2>0.995),方法最低检出限为0.4—1.5μg·kg^-1,最低定量限为1.4—5.0μg·kg^-1.在韭菜、芹菜、番茄、白菜基质中,5、10、50μg·kg^-1添加水平下的加标回收率为60.2%—126.9%,相对标准偏差(RSD)为0.4%—21.6%(n=3).     

Phytoremediation of Cadmium-Contaminated Soils by Rorippa globosa Using Two-Phase Planting (5 pp)

Background Phytoextraction of contaminated soils by heavy metals can provide a great promise of commercial development. Although there are more than 400 species of hyperaccumulators found in the world, phytoremediation technology is rarely applied in field practice for remedying contaminated soils, partially due to low biomass and long growth duration for most of discovered hyperaccumulating plants. In order to enhance the metal-removing efficiency in a year, the two-phase planting countermeasure of phytoextraction by harvesting anthesis biomass was investigated on the basis of the newly found Cd-hyperaccumulator Rorippa globosa (Turcz.) Thell. with 107.0 and 150.1 mg/kg of the Cd accumulation in stems and leaves, respectively, when soil Cd added was concentrated to 25.0 mg/kg. Methods The field pot-culture experiment was used to observe the distribution property of R. globosa aboveground biomass and to examine characteristics of accumulating Cd by the plant at different growth stages. The concentration of Cd in plants and soils was determined using atomic absorption spectrophotometry (AAS). Results and Discussion The results indicated that the total dry stem and leaf biomass of R. globosa harvested at the flowering phase was up to 92.3% of that at its full maturity and the concentration of Cd in stems and leaves harvested at the flowering phase was up to 73.8% and 87.7% of that at the mature phase, respectively. The Cd-removing ratio by shoots of R. globosa harvested at the flowering phase was up to 71.4% of that at the mature phase. It was also found, by observing the growth duration of R. globosa, that the frostless period at the experiment site was twice as long as the growth time from the seedling-transplanted phase to the flowering phase of the hyperaccumulator. Conclusion R. globosa could be transplanted into contaminated soils twice in one year by harvesting the hyperaccumulator at its flowering phase based on climatic conditions of the site and traits of the plant growth. In this sense, the extraction efficiency of Cd in shoots of R. globosa increased 42.8% compared to that of at its single maturity when the plant was transplanted into contaminated soils after it had been harvested at its flowering phase and the plant accumulated Cd from soil at the same extraction ratio at its second flowering phase. Thus, the method of anthesis biomass regulation by the two-phase planting is very significant to increase the Cd-removing efficiency by phytoremediation used in practice over the course of a year. Recommendation and Outlook As for some hyperaccumulators that the growth duration from the seedling-transplanted phase to the flowering phase are short and the concentrations of heavy metals accumulated in their shoots at the flowering phase are high, the efficiency of phytoremediation can greatly be improved using the method of the two-phase planting.     

聚合物涂层纤维材料为固定相填充毛细管气相色谱及其在样品预处理中的应用

1　IntroductionGaschromatography(GC)isoneofthemostpopularseparationmethodsfortheanalysisofvolatilecompounds,andawidevarietyofpolymericmaterialsasthestationaryphases,havebeendeveloped .Incontrasttothesuccessfulapplicationsandsubsequentcommercializationofth…     

Laboratory evidence of natural remobilization of multicomponent DNAPL pools due to dissolution

Mixtures of dense non-aqueous phase liquids (DNAPLs) trapped in the subsurface can act as long-term sources of contamination by dissolving into flowing groundwater. In general, the components of higher solubility are removed more quickly, thus altering the composition of the remaining DNAPL, and possibly leading to changes in its physical properties. Through the development of a simple compositional model, Roy et al. [J. Contam. Hydrol. 2002 (59) 163] showed that preferential dissolution of a mixed DNAPL could potentially result in changes in density and interfacial tension that could subsequently lead to remobilization of an initially static DNAPL pool. The laboratory experiments presented in this next paper provide a proof-of-concept for the previously presented theory, demonstrating and quantifying this process of remobilization. In addition, the experiments provide a data set for evaluation of the model presented by Roy et al. [J. Contam. Hydrol. 2002 (59) 163]. In the four experiments, a DNAPL pool comprised of tetrachloroethene and benzene was created as an open pool overlying glass beads within a water-saturated 2-D flow box. Experiments included rectangular and triangular pools. In each of the experiments, remobilization (as breakthrough) was observed more than 2 weeks after formation of the initial pool. During each experiment, the pool height declined as mass was lost by dissolution, while sampling indicated a decrease in the mole fraction of benzene, the more soluble component. Small protuberances formed along the bottom of the pool as its composition changed with time and the displacement pressure was achieved for various pore throats. Eventually one of the protuberances extended further, forming a finger (breakthrough). In general, the pool emptied as the finger proceeded further into the beads. It was also shown theoretically and experimentally that remobilization will occur sooner for pools with a triangular (pointing down), rather than rectangular, shape. The experimental results were simulated using the model developed by Roy et al. [J. Contam. Hydrol. 2002 (59) 163]. The model matched the observations well, suggesting that it accurately represents the primary mechanisms involved with natural remobilization under the conditions of the study.     

新型规整吸附/光催化偶联催化剂性能研究

在预先成形的金属网上制备规整炭化物载体,载体经TiO2负载、烧结后制成新型规整型吸附/光催化偶联催化剂。以室内空气典型污染物苯为模拟降解对象,研究了该催化剂的光催化活性及活性影响因素。此外,还研究了载体的吸附性、气相的湿度及流速对负载催化剂反应性能的影响。实验结果表明:载体的吸附性对催化剂的反应性能有影响,在苯的初始浓度80mg/m3、光照2h的相同条件下,在两个不同吸附性载体的负载催化剂上,苯的净降解率分别为51.1%和33.56%;气速对催化剂反应性能的影响体现在传质阻力和停留时间上,反应过程存在一个最佳气速;气相的湿度对催化剂的反应性能影响不大,在苯初始浓度300mg/m3、光照2h条件下,气相的相对湿度由33%增至75%,苯的净降解率变化不超过5%。     

SPME-GC/MS法测定垃圾渗沥液中双酚A

建立了固相微萃取-气相色谱质谱联用法测定垃圾渗沥液中双酚A的方法,并用于广州大田山垃圾渗沥液中双酚A含量的测定。对影响萃取的参数进行了优化,实验选用涂层厚度为85μm聚丙烯酸酯(PA)萃取纤维,在搅拌速度为1200r/min、NaCl浓度为20%、pH2.0和室温条件下萃取60min。方法的线性范围为0.1～100μg/L,检出限为0.03μg/L,精密度为6.6%。应用本方法监测了广州大田山垃圾渗沥液中BPA的含量在生物法处理过程中的变化情况。     

影响三沟式氧化沟脱氮效果的2个重要参数

运行周期中反硝化运行和硝化运行的时间比ｔＤＮ／ｔＮ是平衡处理系统反硝化,硝化能力的重要参数,实验室条件下分别比较了ｔＤＮ／ｔＮ为０．２７,０．４０,０．４７,０．７５和１．０的５种不同组合的运行效果。结果表明,当ｔＤＮ／ｔＮ为０．４０时,即硝化能力略大于反硝化潜能时,脱氮效果最好。     

茶叶挥发物对白斑猎蛛觅食行为的影响

为了探明茶树叶片挥发物在白斑猎蛛(Evarcha albaria)选择觅食斑块过程中的作用,采用固相微萃取-气相色谱-质谱联用技术研究了其猎物假眼小绿叶蝉(Empoasca vitis)取食对茶树叶片挥发物释放的影响,同时利用蜘蛛行为观测平台研究了白斑猎蛛在不同味源侧(觅食斑块)的活动行为。结果表明,未损伤叶片(对照)仅释放出微量挥发物,而假眼小绿叶蝉成虫取食后的茶树叶片释放出14种挥发物;雌、雄蛛在进入处理味源(假眼小绿叶蝉取食后的茶树叶片)侧和对照侧的初次选择及进入频次上均无显著差异,但与对照相比,雌、雄蛛在虫害处理叶片中的停留时间显著增加。研究表明,假眼小绿叶蝉取食诱导了茶树叶片挥发物的释放,而挥发物种类和含量的变化造成了白斑猎蛛在不同味源侧停留时间的差异。     

扰动强化污染底泥有机物自净的研究

扰动能够强化水体溶解氧的恢复并加快传质,增强水体的自净作用,有利于水体和底泥COD的降解,是一种常用的污染水体的修复方法。文章通过人工模拟的水体,构建搅拌和曝气两种上覆水扰动条件,研究了在这两种条件下水体中有机物含量以及底泥中微生物量的变化情况,探讨了扰动对水体有机物去除的影响。研究结果表明：（1）与对照情况相比,在搅拌、曝气条件下水中ρ（溶解氧）分别由0.2 mg.L^-1提高到1.0和8.0 mg.L^-1左右;曝气条件下底泥中蛋白含量及细菌数均最高;（2）底泥中w（脱氢酶活性）在搅拌和曝气条件下分别为0.52和0.46μg.g^-1左右;（3）曝气条件下对上覆水中有机物的去除呈现出较好的降解趋势。因此,运用曝气技术既能加速有机物的生化降解,改善水质;又可强化水体溶解氧的恢复,创造了微生物生长繁殖的适宜环境,增强了水体中微生物的活性,促进了水体自净能力的提高,在治理河道污染的应用中具有广阔的前景。     

双负载双金属催化剂催化有机卤化物水相脱卤研究

通过把起相转移作用的聚乙二醇链固载在硅胶上（SiO2-PEG600）,再将聚乙稀吡咯烷酮（PVP）络合双金属Pd-Cu(PVP-PdCl2-CuCl2)后负载其中,制成一种新型双负载双金属水相脱卤催化剂PVP－PdCl2-CuCl2/SiO2-PEG600。以甲酸钠为氢转移试制,在水相中催化有机卤化物脱卤,研究结果表明：反应温度为800℃,Pd∶Cu=2∶1（摩尔比）,反应介质pH≈11.7左右时,该催化剂对芳香氯化物及α－氯代酮、酯具有良好的催化脱氯和重复使用性能。