QuEChERS/超高效液相色谱-串联质谱法同时测定水产品中四溴双酚A与六溴环十二烷

建立了同时测定水产品中四溴双酚A(TBBPA)和六溴环十二烷(HBCD)的超高效液相色谱-串联质谱方法。样品前处理采用QuEChERS方法,均质生物样品用水分散后加乙腈提取,经C_(18)分散固相萃取净化。采用CORTECS~?C_(18)色谱柱(4.6 mm×100 mm×2.7μm)分离,以甲醇-水为流动相进行梯度洗脱,流速为0.7 mL/min。采用电喷雾离子源,在负离子模式下以多反应监测(MRM)方式检测。结果表明,TBBPA和3种HBCD单体在0.5～500μg/L范围内线性良好,相关系数(r)大于0.998,检出限(LOD,S/N=3)和定量下限(LOQ,S/N=10)分别为0.04～0.16μg/kg和0.12～0.55μg/kg。在5、20、50μg/kg加标水平下的平均回收率为74.0%～121%,相对标准偏差(RSD)为0.20%～23%。该方法操作简单、快速、重现性好,适用于水产品中TBBPA和HBCD的快速检测。     

La0.8Ca0.2MnO3纳米线的制备及表征

利用Sol-gel法结合氧化铝模板技术制备了La0.8Ca0.2MnO3纳米线, 并研究了两种热处理方法对 La0.8Ca0.2MnO3纳米线结构和形貌的影响. 快速升温到800 ℃得到的La0.8Ca0.2MnO3纳米线较粗, 其直径大于氧化铝模板的孔径, 而经过缓慢升温到400 ℃预处理再升温到800 ℃得到的La0.8Ca0.2MnO3纳米线, 其直径和氧化铝模板的孔径相当, 都约为35 nm. X射线衍射和透射电镜分析结果表明, 两种方法得到的 La0.8Ca0.2MnO3纳米线都是具有钙钛矿结构的属于单斜晶系的多晶材料.     

D072型树脂脱除过氧化氢中金属阳离子的工艺研究

实验考察D072型阳离子交换树脂在交换柱中脱除过氧化氢中微量金属阳离子的动态行为．通过改变料液流速、高径比、料液中交换离子浓度及料液组成等参数，绘制不同条件下的透过曲线，以此考察D072型树脂对过氧化氢中金属阳离子的动态交换性能，从而确定适宜的工艺条件，为工业化生产提供科学依据．     

Anderson结构铁钼杂多酸稀土盐的合成与结构表征

制备了具有Anderson结构的铁钼杂多酸稀土盐，经元素组成分析、TG和ICP确定其通式为Ln[FeMo6O24H6](Ln^3 =La，Ce，Pr，Nd，Sm，Gd，Dy，Yb)．采用IR，UV,^95Mo-NMR，XRD等方法进行了结构表征，发现在IR光谱图上呈现出羟基和H2O的两个振动谱带，并进行了归属，表明此类杂多酸稀土盐属Anderson结构B型．借鉴TG-DTA、不同温度下的IR和XRD及水溶性实验对Ln[FeMo6O24H6]和(NH4)3[FeMo6O24H6]的热解性质研究表明，此类杂多酸稀土盐的分解温度为350～400℃．比母体酸盐的热稳定性提高了10℃．     

Chemically modified "polar patch" mutants of subtilisin in peptide synthesis with remarkably broad substrate acceptance: designing combinatorial biocatalysts

A significant enhancement of the applicability of the serine protease subtilisin Bacillus lentus (SBL) in peptide synthesis was achieved by using the strategy of combined site-directed mutagenesis and chemical modification to create chemically modified mutant (CMM) enzymes. The introduction of polar and/or homochiral auxiliary substituents, such as X=oxazolidinones, alkylammonium groups, and carbohydrates at position 166 at the base of the primary specificity S(1) pocket created SBL CMMs S166C-S-X with strikingly broad structural substrate specificities. These CMMs are capable of catalyzing the coupling reactions of not only L-amino acid esters but also D-amino acid esters as acyl donors with glycinamide to give the corresponding dipeptides in good yields. These powerful enzymes are also applicable to the coupling of L-amino acid acyl donors with alpha-branched acyl acceptor, L-alaninamide. Typical increases in isolated yields of dipeptides of 60-80 % over SBL-WT (e.g. 0 % yield of Z-D-Glu-GlyNH(2) using SBL-WT-->74 % using S166C-S-(CH(2))(2) NMe(3) (+)) demonstrate the remarkable synthetic utility of this "polar patch" strategy. Such wide-ranging systems displaying broadened and therefore similarly high, balanced yields of products (e.g. 91 % Z-L-Ala-GlyNH(2) and 86 % yield of Z-D-Ala-GlyNH(2) using S166C-S-(3R,4S)-indenooxazolidinone) may now allow the use of biocatalysts in parallel library synthesis.     

芴取代的有机膦化合物的合成及发光性能

合成了以芴为取代基，P原子为核的一类新型有机膦化合物．此类化合物的HOMO值在-5．35～-5．24eV之间．在二氯甲烷中的最大紫外吸收光谱峰值在313～351nm之间，荧光光谱峰值在334～397nm之间．利用此类小分子与纯聚芴进行掺杂，制作了有机电致发光器件．低HOMO值有机膦化合物的引入有效地降低了聚芴发光器件的开启电压，提高了器件的发光效率．     

Syntheses and Crystal Structures of 4,4‘—Diformyl—diphenoxyethane and 4,4’,4‘’—Triformyl—triphenoxytriethylamine

Two title compounds, 4,4'-diformyl-diphenoxyethane (compound 1, C16H14O4)and 4,4',4'-triformyl-triphenoxytriethylamine (compound 2, C27H27NO6), were synthesized by condensation of 4-hydroxybenzaldehyde with 1,2-dichloroethane and tris2-chloroethylamine, respectively in dimethyl formamide in the presence of anhydrous potassium carbonate. The crystal data are: monoclinic, P21/c, a = 7.571(2), b = 12.608(3), c = 7.357(2) ', = 105.823(6)o, V = 675.7(2)'3, Mr = 270.3, Z = 2, Dc = 1.328 g/cm3, F(000) = 284, (MoK = 0.096 mm-1, R = 0.0537 and wR = 0.2189 for compound 1; and monoclinic, P21/n, a = 11.7162(6), b = 9.0042(6), c = 22.908(2) ', = 99.505(1)°, V = 2383.5(3) '3, Mr = 461.50, Z = 4, Dc = 1.286 g/cm3, F(000)= 976, (MoK = 0.091 mm-1, R = 0.0464 and wR = 0.1462 for compound 2. The molecule of compound 1 dialdehyde is located at the crystallographic inversion center nearby the midpoint of C8-C8A single bond. The three chains in the molecule of compound 2 trialdehyde are of non-crystallographic pseudo-C3 symmetry, and each of them is quite planar.     

Synthesis of Novel Dendrimers Containing Amino Acids and Peptides

Dendrimers are known for their well-defined, regular, highly branched architectures with a large number of functional groups1. Recently, dendrimers have been widely researched in different fields, such as molecular light havesting, catalysts, liquid cryst…     

硝基苯在离子液体BMimBF4-H2O中的电还原

采用循环伏安法和恒电位电解法研究了离子液体BMimBF4-H2O 中硝基苯在微铂电极上的电还原特性. 实验表明, 在BMimBF4中, 随着硝基苯和水的浓度变化, 循环伏安曲线的峰电位和峰电流呈现复杂的变化规律; 硝基苯在铂电极上的电还原反应为双分子8 电子3 步骤电化学过程, 第一步反应为准可逆单分子单电子转移步骤, 产生阴离子自由基, 第二步为2 电子转移步骤, 并伴有随后的双分子不可逆自由基偶合化学反应, 主要产物为氧化偶氮苯, 第三步是2 电子转移产生偶氮苯的过程.