4种典型纳米材料对小鼠胚胎成纤维细胞毒性的初步研究

为探讨不同种类纳米材料对原代培养小鼠胚胎成纤维细胞(Mouse embryo fibroblasts,MEF)的毒性效应及作用机制,选择4种典型的纳米材料(纳米碳、单壁碳纳米管、纳米氧化锌、纳米二氧化硅)制备颗粒悬液,设立5个剂量组(5、10、20、50、100μg·mL-1)对BALB/c小鼠MEF细胞进行24、48、72h染毒培养,利用细胞形态学观察和噻唑蓝实验(MTT比色法)检测上述4种纳米材料对MEF细胞活性的影响,同时,测定染毒24h后细胞培养液上清中乳酸脱氢酶(LDH)活性以探讨纳米颗粒对细胞膜完整性的影响.结果显示:1)4种纳米材料均能明显影响MEF细胞的生长形态.染毒24h后,MEF细胞发生不同程度的回缩变形,细胞间隙增大,排列稀疏,胞内颗粒物增多,细胞透明度下降.2)纳米碳、纳米氧化锌、纳米二氧化硅对MEF细胞增殖的抑制作用和对细胞膜完整性的损伤作用均随染毒剂量的升高而增强,具有明显的剂量-效应关系,其半数致死浓度(24h-IC50)分别为21.85、21.94、461.10μg·mL-1;碳纳米管组的剂量-效应之间不呈对数线性关系,未能得出其24h-IC50.3)在不同染毒剂量水平上,4种纳米材料的毒性对比差异显著:低剂量水平上纳米碳与碳纳米管的毒性强于纳米氧化锌和纳米二氧化硅,随着剂量的升高纳米氧化锌的细胞毒性升高最为显著.结果提示,纳米材料能够对MEF细胞造成毒性损伤,破坏细胞膜的完整性可能只是作用途径之一;纳米材料的毒性可能受粒径、形状、化学组成等许多因素的影响.     

Packed in-tube solid phase microextraction with graphene oxide supported on aminopropyl silica: Determination of target triazines in water samples

On-line in-tube solid phase microextraction (in-tube SPME) coupled to high performance liquid chromatography and tandem mass spectrometry (HPLC-MS/MS) was successfully applied to the determination of selected triazines in water samples. The method based on the employment of a packed column containing graphene oxide (GO) supported on aminopropyl silica (Si) showed that the extraction phase has a high potential for triazines extraction aiming to its physical-chemical properties including ultrahigh specific surface area, good mechanical and thermal stability and high fracture strength. Injection volume and loading time were both investigated and optimized. The method validation using Si-GO to extract and concentrate the analytes showed satisfactory results, good sensitivity, good linearity (0.2–4.0 µg L^?1) and low detection limits (1.1–2.9 ng L^?1). The high extraction efficiency was determined with enrichment factors ranging from 1.2–2.9 for the lowest level, 1.3–4.9 intermediate level and 1.2–3.0 highest level (n = 3). Although the analytes were not detected in the real samples evaluated, the method has demonstrated to be efficient through its application in the analysis of spiked triazines in ground and mineral water samples.     

MCM-41介孔分子筛的合成及其对铜离子的吸附性能简

以微硅粉为硅源,CTAB和PEG-6000为模板剂,合成MCM-41介孔分子筛。采用XRD、N₂吸附-脱附曲线、FTIR以及TEM表征了其结构、比表面积、孔径分布及晶体形貌,并且以该样品为吸附剂,对含Cu²⁺的溶液进行了静态吸附实验。结果表明,以微硅粉为硅源成功合成了具有典型六方排列孔道结构的MCM-41,其比表面积为869.5 m²/g,孔容为0.97 cm³/g,平均孔径为3.3 nm;溶液pH为5~6时,MCM-41对Cu²⁺的去除效果最好;MCM-41对Cu²⁺的最大吸附吸附容量36.3 mg/g;MCM-41对Cu²⁺的吸附性能符合Langmuir吸附方程的特征。动力学研究表明,该过程符合准二级动力学模型。     

Hydrothermal liquefaction phase behavior of microalgae & model compounds in fused silica capillary reactor

A fused silica capillary reactor combined with a heating/cooling stage, a microscope and a digital camera were used to investigate phase behavior during the hydrothermal liquefaction of microalgae (Dunaliella tertiolecta) and model compounds, including soya protein and glycine, starch, glucose and xylose, stearic acid and palmitic acid. Bubbles were generated at 246°C and disappeared at 360°C upon heating when Dunaliella tertiolecta used as feedstocks. Moreover, liquid products were generated at 300°C upon heating and oily liquid products began to separate out at 250°C upon cooling. The phase behavior of soya protein was similar to that of the Dunaliella tertiolecta. Meanwhile, there only observed the bubbles generation during hydrothermal liquefaction of glycine. Heating the starch, glucose and xylose above 350°C generated black solids from carbonization. Stearic acid and palmitic acid only had the process of melting, dissolution, dispersion and precipitation.     

二乙烯三胺改性聚多巴胺包覆硅胶吸附日落黄

采用二乙烯三胺(DETA)改性聚多巴胺(PDA)包覆硅胶(SG)得到吸附剂SG@DETA/PDA。通过FTIR、SEM和氮气吸附-脱附等技术对SG@DETA/PDA进行了形貌和结构表征,并考察了其对阴离子染料日落黄的吸附性能。表征结果显示,SG@DETA/PDA表面有PDA微球团聚形成的较为致密的包覆层,其比表面积和孔体积均比吸附剂SG@PDA有小幅提高。实验结果表明:SG@DETA/PDA吸附日落黄的最佳工艺条件为溶液p H 2.0、吸附时间2.0 h、初始染料质量浓度150 mg/L,在上述最佳工艺条件及298 K温度条件下SG@DETA/PDA对日落黄的吸附容量为175.56 mg/g。SG@DETA/PDA吸附日落黄的过程可以分别用准二级动力学方程和Langmuir等温吸附方程很好地拟合,该吸附过程主要是通过静电作用的单分子层吸附,是一个吸热自发的熵增过程。     

An impingement plate method to detect deposits of pyrethroid insecticides

Abstract

A silica gel impingement plate for monitoring pyrethroid deposits in environmentally sensitive areas is described. The plate is simple, commercially available, and inexpensive. A residue analysis method is given for deltamethrin deposits with 83.3% mean recovery and a minimum quantifiable limit of 0.005 μg/plate. Pyrethroid deposits are strongly adsorbed to the silica gel, which prevents wash‐off by rainfall and slows photodegradation. In two field experiments, deltamethrin was readily detected 3 weeks after direct spray applications at 6 and 10 g ai/ha. Deltamethrin dissipation on the plates was first‐order with a half‐life of 2.9 ‐ 3.7 d. Photoisomers of deltamethrin were also detected on the plates and the ratio of photoisomers to deltamethrin increased over time. This ratio will indicate the age of deposits in monitoring situations.     

植物根瘤内痕量Frankia DNA的提取及鉴定

建立了一种简捷、快速植物根瘤内痕量Frankia DNA的提取方法,即采集自然态下根瘤,剥离瘤瓣,取瘤瓣尖经液氮研主民粉末,以20g/L CTAB（十六烷基三甲基溴化铵）消化胞壁,然后以d=5-10μm的石英粉吸附DNA,再以无菌去离子蒸馏水释放DNA,所获DNA产率及纯度较酚／氯仿法好。经对辽宁沙棘、色赤杨根瘤的瘤内痕量Frankia DNA及体外培养的9种Frankia菌株DNA分纯,并用于酶切及PCR,获满意结果。图3参12     

固相萃取-GC/MS法测定地表水中3-甲基吲哚

采用微球硅胶键合C_(18)固相萃取柱萃取水样中的3-甲基吲哚,并用气质联用法测定,方法在0 mg/L~10.0 mg/L范围内线性良好,方法检出限为0.2μg/L。空白水样3个质量浓度水平的加标回收率为89%~94%,7次测定结果的RSD为2.3%~6.9%。用该方法测定7个实际地表水样品,其中4个地表水样品检出3-甲基吲哚,地表水样的加标回收率为81.5%~97.0%。     

红外光谱法测定粉尘中游离二氧化硅综述

全面地回顾了国内外红外光谱法测定粉尘中游离二氧化硅的研究成果。系统而重点地介绍了溴化钾压片法、粉尘滤膜样品重沉积和采样滤膜直接测定技术,分析了样品粒度、标准石英物质和矿物干扰物对测定结果的影响及干扰消除方法;还介绍了国外对红外光谱法与Ｘ－射线衍射法进行比较性研究的结果和动态,并得出结论。文章所列参考文献对本领域研究人员和基层检测人员具有很高的参考价值。     

氯化钠/纳米疏水二氧化硅超细干粉制备及灭火性能研究

选用氯化钠为基体制备金属火灾超细干粉灭火剂。应用反溶剂法对其改性,使纳米疏水二氧化硅吸附在氯化钠晶体表面,其中分散剂为PEG-1000。结果表明,纳米疏水二氧化硅的添加有利于细化氯化钠颗粒,但过量的添加会起反作用,最佳用量为3 wt%左右,平均粒径为2.18μm。镁片灭火实验证明超细复合干粉的灭火性能明显好于传统氯化钠灭火剂(商用D类灭火剂),纳米疏水二氧化硅最佳添加量为3 wt%,此时灭火时间仅需传统灭火剂的一半。最后利用FDS5.0模拟干粉颗粒与燃烧火焰作用过程,模拟结果表明干粉覆盖对火焰具有一定的抑制效果,并分析了复合干粉灭火机理。