Template‐Free Hydrothermal Synthesis of Mesoporous MgO Nanostructures and Their Applications in Water Treatment

The controlled synthesis of Mg(OH)₂ nanowires and microflowers composed of nanoplates was successfully achieved by a template‐free hydrothermal synthetic method. It was found that the reaction medium played a crucial role in the morphological control of the precursor nanostructures. The high polarity of water molecules favored the polar growth of the precursor, resulting in the formation of nanowires with a diameter of 80 nm, whereas a mixed water/ethanol medium with a lower degree of polarity led to the formation of microflowers. Moreover, mesoporous MgO nanostructures could be obtained by further annealing these as‐prepared precursors in air at 500 °C for 2 h. During thermal treatment, the wire‐ and flower‐like morphologies were retained. Porosity formation was due to thermal decomposition of Mg(OH)₂ and release of H₂O. Both the mesoporous MgO nanowires and microflowers showed superior ability of adsorbing the organic dye methyl orange, and thus they are promising candidates for polluted water treatment.     

高效液相色谱-串联质谱法快速测定6类食品中增效醚的残留

建立了水果、蔬菜、粮谷、油料、动植物脂类、动物源性食品等6类食品中增效醚残留量快速测定的液相色谱-质谱/质谱(LC-MS/MS)方法。样品盐析并除水后,用三氯甲烷提取,氟罗里硅土填料固相萃取柱净化,丙酮-三氯甲烷混合溶剂洗脱,以乙腈-0.1%甲酸为流动相,在Zobax SB C18液相色谱柱完成分离,并于电喷雾正离子多反应监测模式下质谱测定。考察了提取溶剂、净化方法、柱容量、仪器条件、基质效应对分析结果的影响。增效醚质量浓度在0.5～100μg/L范围内,线性相关系数(r)为0.9976,方法定量限(LOQ)为10μg/kg。17种食品基质添加LOQ、低MRL、2倍MRL、高MRL 4个不同浓度水平时,回收率在80.3%～96.3%之间,相对标准偏差为2.7%～14%,方法可以满足多种食品基质中增效醚残留量的定性和定量检测要求。     

Hydrothermal Synthesis,Crystal Structure and Magnetic Property of a New Co（Ⅱ） Complex：[Co（4,4＇-bpy）_2（H_2O）_2（4-FBA）_2]·（4,4＇-bpy）

A new complex [Co(4,4'-bpy)2(H2O)2(4-FBA)2]·(4,4'-bpy)(1) has been hydro-thermally synthesized using cobalt,4,4'-bipyridyl(4,4'-bpy) and 4-fluorobenzoic acid(4-HFBA),and characterized by thermal analysis,single-crystal X-ray diffraction and magnetic property.The complex crystallizes in the triclinic system,space group P,Z = 1.Crystal data:C54H44CoF2N8O6,Mr = 997.90,a = 9.134(2),b = 11.555(2),c = 12.867(3) ,α = 66.02(3),β = 77.96(3),= 73.11(3)°,V = 1180.9(4) 3,Dc = 1.403 g/cm3,μ(MoKα) = 0.433 mm-1,F(000) = 517,the final R = 0.0633 and wR = 0.1171 for 2152 observed reflections(I > 2σ(I)).The title complex is assembled into 1D supramolecular chains parallel to [001] based on the adjacent molecular ··· stacking interactions and hydrogen bonds.The variable temperature magnetic measurements show a weak ferromagnetic behavior over 300-160 K followed by antiferromagnetic behavior below 160 K for the title complex.     

液相色谱-四极杆飞行时间质谱法快速测定草莓中6种植物生长调节剂的残留量

建立了高效液相色谱-四极杆飞行时间串联质谱(HPLC-Q TOF MS)快速检测草莓中2,4-滴、对氯苯氧乙酸、3-吲哚丁酸、氯吡脲、脱落酸、玉米素6种植物生长调节剂的分析方法。样品采用QuEChERS方法(Quick, Easy, Cheap, Effective, Rugged and Safe method)进行前处理(乙腈提取,C18吸附剂净化),采用Eclipse XDB-C8色谱柱(150 mm×4.6 mm, 5 μm),以乙腈-5 mmol/L乙酸铵-0.1%(v/v)甲酸水溶液为流动相,梯度洗脱,Q TOF MS电喷雾负离子模式分析检测。在全扫描采集模式下,以准分子离子峰的峰面积定量,以化合物的精确质量数定性。在Target MS/MS采集模式下,通过碎片离子的精确质量数进一步确证化合物。各化合物在0.005～1.0 mg/L范围内均呈现良好的线性关系,相关系数均大于0.99。6种化合物的检出限为1～5 μg/kg,添加回收率为87%～107%,相对标准偏差(RSD)均小于10%(n=6)。本方法简便快捷,选择性好,灵敏度高,可满足国内外现行法规的限量要求。     

Rapid Sample Pretreatment,Identification and Determination of Active Constitutents in Water‐soluble Radix isatidis Extract via MAE,ESI‐MS and RODWs‐HPLC

In this study, we successfully studied water‐soluble extract from Radix isatidis. Optimized conditions of MAE were listed, the sample can be extracted completely in 10 minutes under microwave power of 400W and solid/liquid ratio of 1:80. Active compounds in water‐soluble extract from R. isatidis were identified with HPLC‐DAD/ESI‐MS, these compounds followed by cytidine, uridine, guanosine, (R,S)‐goitrin and adenosine. RODWs–HPLC as a new sensitive chromatography were also first proposed and investigated, we favoringly used this method for simultaneous determination of these active constitutents in water‐soluble R. isatidis extract. Chromatographic separation was performed on a Diamonsil C18 column (5 μm, 150 mm × 4.6 mm) with a mobile phase gradient consisting of methanol and water at a flow‐rate of 1.0 mL/min, detection wavelengths 240, 250, 260 and 270 nm, the retention times of the tested five compounds were about 4.2, 5.8, 11.1, 14.2 and 20.8 min respectively, the limits of detection were 15, 12, 20, 5.8 and 24 ng/mL for cytidine, uridine, guanosine, (R,S)‐goitrin and adenosine respectively, their linear ranges were between 0.045 and 350 μg/mL with correlation coefficient (R) of 0.9998‐0.9999. The relative standard deviations (RSDs) of intra‐day and inter‐day assays were 0.30‐2.36% and 0.86‐2.54% respectively. Extraction recoveries were 94.25‐106.21%. This novel analytical method was shown to be simple, low‐cost, sensitive and reliable for multiple components in complex or undeveloped materials via MAE, ESI‐MS and RODWs‐HPLC.     

新型氨基甲酸乙酯人工抗原的分析表征方法研究

采用1-(3-二甲氨基丙基)-3-乙基碳二亚胺方法合成氨基甲酸乙酯(Ethyl carbamate,EC)新型人工抗原.将衰减全反射红外光谱法(ATR-FTIR)应用于人工合成抗原的表征分析,并结合荧光光谱分析EC人工抗原的偶联效果以及载体蛋白质分子的二级结构变化;通过质谱结合紫外光谱、电泳方法进行人工抗原的系统表征,计算新型人工抗原中半抗原分子与载体蛋白质分子的偶联比.结果表明:合成路线合理,成功获得了氨基甲酸乙酯新型人工抗原.人工抗原分子的α-螺旋、β-折叠和β-转角结构与载体蛋白质分子相比含量发生变化,人工抗原的荧光相图满足线性型态变迁关系,符合“二态模型”.氨基甲酸乙酯人工抗原分析表征的红外衰减全反射方法、基质辅助激光解析飞行时间质谱法获得的检测结果与其它光谱方法、电泳方法表征结果一致,获得人工抗原的偶联比为15∶1～19∶1,EC新型人工抗原免疫小鼠抗血清的效价为1∶25600.     

石墨烯包覆碳纳米管-硫(CNT-S)复合材料及锂硫电池性能

针对锂硫电池研究与实际应用中遇到的主要问题, 本文通过一种简单有效的水热法还原氧化石墨烯对商用碳纳米管-硫(CNT-S)纳米复合材料进行包覆, 形成一种可有效抑制多硫聚合物扩散的石墨烯包覆结构。X射线衍射(XRD), 扫描电子显微镜(SEM)表征结果表明硫均匀地负载在碳纳米管上, 并且在CNT-S复合材料外表面包覆有一层石墨烯。电化学测试结果表明, 这种包覆结构能显著提高CNT-S复合材料的锂硫电池性能。     

双四唑胺和钐构筑的含单核结构的配合物的水热合成和晶体结构

以双四唑胺(H₂BTA)、氯化钐为原料,通过水热法合成了一个双四唑胺合钐配合物[Sm₂(BTA)₃·(H₂O)₁₀]·5H₂O(H₂BTA=双四唑胺)。X-射线单晶衍射表征了这个配合物属于三斜晶系,P1空间群。在配合物中,两种不同的Sm³⁺离子与双四唑胺的2个螯合N原子和水分子配位形成2种八配位的四方反棱柱结构的单核配合物单元。在2种单核配合物单元和结晶水分子之间,存在着O-H…N,O-H…O和N-H…N 3种不同的氢键,形成三维超分子结构     

HPLC-AFS联用测定海产品中砷的形态

建立了高效液相色谱-原子荧光分光光度法测定海产品中无机砷(As V,AsⅢ)、有机砷(DMA,MMA,AsB)含量的方法.样品经含10％(体积分数)HC1的提取液振荡提取、离心分离、二路形态分析预处理、高效液相色谱分离,用原子荧光光度计检测As(Ⅲ),DMA,MMA,As(v);四路条件(过氧化氢氧化和开启紫外灯)形态分析预处理装置处理,高效液相色谱分离,原子荧光光度计测定AsB.As(Ⅲ)线性范围为0～100.00 μg/L,r2=0.9997;DMA线性范围为0～100.00 μg/L,r2=0.9993;MMA线性范围为0～100.00 μg/L,r2=0.9990;As(Ⅴ)线性范围为0～100.00 μg/L,r2=0.999 1;AsB线性范围为0～200.00 μg/L,,r2=0.9994.3个样品加标回收率为As(Ⅲ)86.7％～89.4％,DMA 111.2％～117.0％,MMA 109.7％～111.6％,As(Ⅴ) 83.8％～90.7％,AsB 88.3％～90.4％.用该方法测定虾仁(干)5个价态测定结果的相对标准偏差为3.07％～9.93％(n=6).5个价态的检出限(S/N=2)为As(Ⅲ)0.29 μg/L,DMA 0.36 μg/L,MMA 0.27 μg/L,As(V) 0.56 μg/L,AsB l.46 μg/L.该方法适用于海产品中As(Ⅲ),DMA,MMA,As(V),AsB含量的测定.     

模板分子诱导的微孔镧系-2-羧基肉桂酸超分子配合物的合成与结构

由水热法合成了2个微孔镧系超分子配合物[Ln(CCA)(OH)(phen)(H2O)]n·n(phen)·nH2O(Ln=Yb,1;Er,2;H2CCA=2-羧基肉桂酸;phen=1,10-菲啰啉),并用元素分析、IR及X-射线单晶衍射对其进行了表征。晶体结构研究表明,2个配合物都是由配体2-羧基肉桂酸连接而形成的一维双链结构,该链状结构通过氢键和π-π堆积作用扩展为具有微孔结构的超分子。1,10-菲啰啉在微孔结构的形成过程中起到了模板剂的作用。