微波消解-电感耦合等离子体质谱法测定粮食中12种重金属元素

粮食样品用硝酸-过氧化氢微波消解处理,采用电感耦合等离子体质谱法测定样品溶液中12种重金属元素(砷、铅、镉、硒、铬、铊、锰、镍、铜、铀、钴、钒)的含量。采用内标法消除基体的影响。方法的检出限(3S/N)在0.092~17.5pg·g-1之间。方法的加标回收率在88.1%~118%之间,相对标准偏差(n=5)小于6.0%。方法用于鸡肉标准物质(GBW 10018)中重金属含量的测定,测定值与认定值相符。     

Tuning of NaTaO_3 Band Structure through Mn~（2＋） Ion Doping and the Enhanced Visible Light Response

Pure and Mn-doped NaTaO3 nanoparticles were synthesized by a simple hydro- thermal method. XRD and XPS results suggested that manganese ions were successfully doped into the NaTaO3 crystalline in Mn2＋ state. UV-vis diffuse reflectance spectra revealed the obvious red-shift in the series of manganese doped NaTaO3 nanoparticles, resulting in a decrease in the band gap of NaTaO3 with the increase of Mn2＋ doping concentration. The photo-degradation experiment indicated that manganese doped NaTaO3 showed good photocatalytic performance and methylene blue（MB） degradation is improved with lower doping concentration of manganese ions under visible light. The simulation of energy band structure by density functional theory unfolded that the substitution of Ta5＋ ions by Mn2＋ ions resulted in an intermediate band（IB） below the bottom of the conduction band（CB）, which was mainly attributed to the state of Mn 3d.     

Fe-Co Alloyed Nanoparticles Catalyzing Efficient Hydrogenation of Cinnamaldehyde to Cinnamyl Alcohol in Water

Selective hydrogenation of C=O against the conjugated C=C in cinnamaldehyde (CAL) is indispensable to produce cinnamyl alcohol (COL). Nonetheless, it is challenged by the low selectivity and the need to use organic solvents. Herein, for the first time, we report the use of Fe-Co alloy nanoparticles (NPs) on N-doped carbon support as a selective hydrogenation catalyst to efficiently convert CAL to COL. The resultant catalyst with the optimized Fe/Co ratio of 0.5 can achieve an exceptional COL selectivity of 91.7 % at a CAL conversion of 95.1 % in pure water medium under mild reaction conditions, ranking it the best performed catalyst reported to date. The experimental results confirm that the COL selectivity and CAL conversion efficiency are, respectively promoted by the presence of Fe and Co, while the synergism of the alloyed Fe-Co is the key to concurrently achieve high COL selectivity and CAL conversion efficiency.     

液相色谱-四极杆-静电轨道阱高分辨质谱法测定保健食品中11种磷酸二酯酶抑制剂

保健食品样品用50%(体积分数)甲醇溶液超声提取15 min,提取液用水定容至50.0mL,离心,取上清液,经0.22μm微孔滤膜过滤,采用液相色谱-四极杆-静电轨道阱高分辨质谱法测定滤液中11种磷酸二酯酶抑制剂的含量。以Waters HSS T3色谱柱为固定相,以不同体积比的0.1%(体积分数)甲酸溶液和乙腈的混合液为流动相进行梯度洗脱,质谱分析中采用电喷雾离子源正离子模式和全扫描模式。11种磷酸二酯酶抑制剂的质量浓度均在2~100μg·L^-1内与其对应的峰面积呈线性关系,测定下限(10S/N)为0.02~0.5μg·L^-1。以空白样品为基体进行加标回收试验,所得回收率为75.7%~98.9%,测定值的相对标准偏差(n=6)为5.9%~14%。     

Temperature-dependent structural changes of[Bmim]FeCl4 magnetic ionic liquid characterized by an in-situ X-ray absorption fine structure

The temperature-dependent structural changes in 1-butyl-3-methylimidazolium tetrafluoride([Bmim]FeCl4)magnetic ionic liquid(MIL)were investigated by using in-situ X-ray absorption fine structure(XAFS)combined with Raman spectroscopy and DFT calculations.XAFS re sults revealed that the coordination number and bond length of Fe-Cl in the anion of[Bmim]FeCl4 MIL decreased with increments in temperature.These results directly reflected the dissociation of tetrahedral structure[FeCl4]^-,and the formation of bridge-chain[Fe2 Cl5]^+,and[FeCl2]^+species in the anion of[Bmim]FeCl4 MIL.These behaviors indicated that[FeCl4]^-dissociation was endothermic,and was promoted by increased temperature.The results obtained through XAFS were in agreement with those obtained through Raman spectroscopy and DFT calculations.     

富马酸丙酚替诺福韦合成工艺改进

对富马酸丙酚替诺福韦的合成工艺进行了改进,以干燥的替诺福韦为起始原料,与亚磷酸三苯酯反应得到(R)-9-(2-(苯基磷酰基甲氧基)丙基)腺嘌呤（3）; 3被氯化亚砜氯代得(R)-9-(2-(((苯基)(氯代)(磷酰基)甲氧基)丙基)腺嘌呤（4）; 4与L-丙氨酸异丙酯盐酸盐缩合得9-((R)-2-(((S)-((1-(异丙氧基羰基)乙基)氨基)苯氧基磷酰基)甲氧基)丙基)腺嘌呤（5）; 5经析晶纯化得9-((R)-2-(((S)-（((S)-1-(异丙氧基羰基)乙基)氨基)苯氧基磷酰基)甲氧基)丙基)腺嘌呤（丙酚替诺福韦,6）; 6与富马酸成盐得富马酸丙酚替诺福韦,其结构经¹H NMR, ¹³C NMR, MS(ESI),元素分析和XRD确证。按改进工艺进行公斤级规模放大,产品总收率达到32.2%,化学纯度99.92%,非对映异构体纯度99.99%。     

Recent Advance of Tellurium for Biomedical Applications

Tellurium(Te) nanomaterials have aroused a wide interest in semiconductor, thermoelectric, piezoelectric, as well as biomedical applications. The last decades of reports indicated a major nanostructure of one-dimensional (1D) Te on account of its inherent structural anisotropy. Two-dimenional(2D) Te has been newly developed and drawn a lot of interests recently. This review presents the intrinsic biological potential of Te-based nanomaterials and summarizes their up-to-date advance in phototherapy and reactive oxygen species(ROS)-related applications in the biomedical field.     

广义神经传播方程的整体吸引子

使用Galerkin方法,结合Sobolev空间理论和不等式技巧,给出了广义神经传播方程解的存在唯一性定理,然后利用吸引子存在性定理,采用半群方法证明了方程整体吸引子的存在性.     

新型双核铜金属配合物为中性载体的硫氰酸根离子高选择性电极的研究

研制了基于N,N'-亚乙基(μ-5,5-亚甲基-二水杨醛根)(乙酰丙酮根)合二铜(II) [Cu₂(II)-MDSBAE]金属配合物为中性载体的阴离子选择性电极. 试验表明, 以Cu₂(II)-MDSBAE金属配合物为中性载体的电极对SCN^－具有良好的电位响应特性, 且呈现反Hofmeister行为,其选择性序列为: SCN^－＞Sal^－＞I^－＞ClO₄^－＞NO₃^－＞Br^－＞NO₂^－＞Cl^－≈SO₃^2－＞SO₄^2－. 在pH 5.0的磷酸盐缓冲体系中, 电极电位呈现近能斯特响应, 线性响应范围为1.0×10^－6～1.0×10^－1 mol/L, 斜率为－53. 6 mV/dec (25 ℃), 检测下限为8.1×10^－7 mol/L. 用交流阻抗研究了电极的响应机理, 并用紫外可见光谱技术测定了电极载体与SCN^－, Sal^－, I^－, ClO₄^－和NO₃^－离子间的配位数及缔合常数. 将该电极用于实验室废水和工业废水中硫氰酸根的检测, 其结果令人满意.     

基于同步辐射原位CT的水牛角结构性能关系研究

为探究水牛角的结构性能关系,基于上海同步辐射光源搭建了高分辨原位CT系统,对水牛角角鞘进行初始表征和准静态压缩下的实时表征,并通过Top-Hat方法提取了角鞘内孔洞三维形貌.结果显示,水牛角角鞘孔隙率在1％左右,椭圆柱状孔洞沿牛角生长方向排列成线,首尾相连却并未连通,均匀分布在波浪状片层之间.孔洞特征椭球的轴长分布满足...