SO42-/SnO2-硅藻土型固体酸的制备及其对正丁酸与异戊醇的催化酯化

采用质量比为1∶3的SnCl₄·5H₂O和硅藻土制备的硅藻土Sn(OH)₄溶胶,70 ℃老化12 h,90 ℃干燥12 h、3.0 mol/L硫酸浸渍3 h、550 ℃焙烧3.5 h,制备了SO₄^2-/SnO₂硅藻土型固体酸催化剂。 利用IR、 XRD、TG测试技术表征了催化剂的理化性质。 用于催化正丁酸与异戊醇的酯化反应,当n（异戊醇）∶n（正丁酸）=1.4∶1、催化剂用量为反应物总质量的2.5%、10 mL苯、反应时间70 min时,酯收率为97.7％。 结果表明,该催化剂兼具多元氧化物型固体酸和硫酸酸化改性天然粘土固体酸催化剂的优点,催化活性高,成本低廉、制备方法简单并可适当回收循环使用。     

Complexing capacity profiles of naturally occurring ligands in Tempranillo wines for Cu and Zn: an electroanalytical approach for cupric casse

Complexing capacity of naturally occurring ligands in Vitis vinifera (Tempranillo variety) wines has been studied with respect to two target metals (Cu and Zn) by differential pulse anodic stripping voltammetry (DPASV). Eight commercial wines of two certified brands of origin (CBO) and a young wine along its vinification process were monitored. Conditional stability constants and total complexing ligand(s) concentration(s) have been calculated for both metals. Discussion of the particular electrochemical responses for Cu and Zn for all samples is presented. A follow-up of the Cu stripping response allowed differentiating a commercial wine from one under processing related to the cupric casse phenomenon. Interaction of Cu with two molecular forms of cyanidin has been theoretically modeled at natural wine pH.     

新型杀菌农药去氢枞酸铜乳油有效成分分析

本文选用高效液相色谱法测定去氢枞酸的含量，从而可以推算去氢枞酸铜的含量。此分析方法的回收率为98％～101％，变异系数为2．96％。     

四(三苯基氧化膦)二氯稀土(Ⅲ)-三氯化铜(Ⅱ)配合物的合成和谱学性质

合成了通式为[LnCl_2(Ph_aPO)_4][CuCl_3](Ln=La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Y)的12种新配合物,X射线衍射结构分析证实[GdCl_2(Ph_2PO)_4][CuCl_3]中Gd(Ⅲ)为六配位畸变八面体形,Cu(Ⅱ)为三配位平面三角形.测定了所有配合物的红外光谱、~(31)P NMR和Cu(Ⅱ)的顺磁共振谱,并对[LnCl_2(Ph_3PO)_4][CuCl_3]的生成进行了讨论.     

用于CO2加氢合成甲醇超细CuO-ZnO/SiO2-ZrO2催化剂

用溶胶－凝胶法制备了ＣｕＯ－ＺｎＯ／ＳｉＯ２－ＺｒＯ２复合氧化物催化剂，使用ＩＲ，ＸＲＤ，ＴＥＭ和ＢＥＴ等手段对催化剂的结构及表面性能进行了表征，考察了ＺｒＯ对该体系的表面性质，结构，ＣｕＯ分散状态以及二氧化碳加氢合成甲醇的催化性能的影响。结果表明，该体系催化剂的比表面积大，活性组分分散均匀。     

长周期光纤光栅对铜离子的检测研究

利用有机反应在长周期光纤光栅表面制备了一层高分子材料敏感膜,用扫描电子显微镜(SEM)、X射线型能谱仪(EDX)等检测手段对高分子敏感膜层进行了分析表征,并利用敏感膜时溶液中的铜离子进行了光学检测。结果表明,该高分子敏感膜能够较好地确定铜离子的存在,证明了利用长周期光纤光栅对铜离子进行检测是可行的。     

Development and Validation of a LC-MS/MS Technique for the Analysis of Short Chain Fatty Acids in Tissues and Biological Fluids without Derivatisation Using Isotope Labelled Internal Standards

The gut microbiota is critical to the maintenance of physiological homeostasis and as such is implicated in a range of diseases such as colon cancer, ulcerative colitis, diabetes, cardiovascular diseases, and neurodegenerative diseases. Short chain fatty acids (SCFAs) are key metabolites produced by the gut microbiota from the fermentation of dietary fibre. Here we present a novel, sensitive, and direct LC-MS/MS technique using isotopically labelled internal standards without derivatisation for the analysis of SCFAs in different biological matrices. The technique has significant advantages over the current widely used techniques based on sample derivatization and GC-MS analysis, including fast and simple sample preparation and short LC runtime (10 min). The technique is specific and sensitive for the quantification of acetate, butyrate, isobutyrate, isovalerate, lactate, propionate and valerate. The limits of detection were all 0.001 mM except for acetate which was 0.003 mM. The calibration curves for all the analytes were linear with correlation coefficients r² > 0.998. The intra- and inter-day precisions in three levels of known concentrations were <12% and <20%, respectively. The quantification accuracy ranged from 92% to 120%. The technique reported here offers a valuable analytical tool for use in studies of SCFA production in the gut and their distribution to host tissues.     

对甲苯磺酸催化合成丁酸丁酯的研究

丁酸丁酯是无色至淡黄色透明油状液体,有成熟香蕉似水果香气.稀释时为菠萝和朗姆酒香气及稀奶油滋味.天然品存在于苹果、香蕉、葡萄、梨、草莓、李、西番果等中.主要用以配制苹果、香蕉、梨和奶油等型香精,是我国GB2760-86规定允许使用的食用香料;也可用于有机合成和用作溶剂.通常它是在硫酸催化下由丁酸和正丁醇酯化反应而得[1-2],硫酸虽活性高,价廉,但选择性差,产品质量不好,设备腐蚀严重,同时产生大量废液,污染环境.因此人们寻求更优良的催化剂来代替硫酸,已发现强酸性阳离子交换树脂、磺酸树脂、固体超强酸、杂多酸以及过渡金属硫酸铜、氯化铁等均可作为酯化反应的催化剂[3-8].但用固体酸催化合成丁酸丁酯至今未见报道.对甲苯磺酸是一种强有机酸,无氧化性,无碳化作用,作为酯化反应的催化剂时,具有活性高,选择性好,产品纯度高,不腐蚀设备,减少污染等优点[9-10].本文利用对甲苯磺酸作催化剂合成丁酸丁酯,讨论了影响反应的因素,在适当的合成条件下,酯化率可达97.8%.     

CuSO4 Micro-crystal Lattice Produced by Microcontact Printing

ＩｎｔｒｏｄｕｃｔｉｏｎＴｈｅ ｐｒｅｐａｒａｔｉｏｎｏｆｍｉｃｒｏ ｐａｒｔｉｃｌｅｌａｔｔｉｃｅｗｉｔｈｓｔｒｉｃｔｓｉｚｅｓａｎｄｓｐａｃｅｃｏｎｔｒｏｌｉｓａｎｉｍｐｏｒｔａｎｔｐｒｏｂｌｅｍｔｏｂｅｓｏｌｖｅｄｕｒｇｅｎｔｌｙｉｎｍａｎｙｈｉｇｈ ｔｅｃｈｆｉｅｌｄｓ .Ｔｒａｄｉ ｔｉｏｎａｌｍｉｃｒｏ ｆａｂｒｉｃａｔｉｏｎｍｅｔｈｏｄｉｓｐｈｏｔｏｌｉｔｈｏｇｒａｐｈｙ ,ｂｕｔｉｔｉｓｕｎａｂｌｅｔｏｐｒｏｄｕｃｅａｎｙｐａｔｔｅｒｎｓｏｎａｃｕｒｖｅｄｓｕｒｆａｃｅａｎｄｄｉｆｆｉｃ…