阿斯美胶囊中四种组分的高效液相色谱分析

建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ８，５μｍ，２００ｃｍ×４０ｍｍＩＤ，流动相为体积分数０５％的三乙胺溶液（磷酸调节ｐＨ５５）＋乙腈＋甲醇（５５０＋３６８＋８２），检测波长为２６４ｎｍ，线性范围分别为：氨茶碱３１２５～２５０ｍｇ／Ｌ，γ＝０９９９６，盐酸甲氧非那明１５６２５～１２５０ｍｇ／Ｌ，γ＝１００００，马来酸氯苯那敏２５～２００ｍｇ／Ｌ，γ＝０９９９９，那可汀８７５～７００ｍｇ／Ｌ，γ＝０９９９９；回收率（ｎ＝３）分别为１０１２％，１００８％，９９９％，９９５％；精密度：日内平均ＲＳＤ（ｎ＝６）分别为０７％，０４％，０４％，０６％；日间平均ＲＳＤ（ｎ＝３）分别为１０％，１０％，１１％，１２％。     

烷基多苷的分析测定

ＧＣ、＾１Ｈ－ＮＭＲ和＾１３Ｃ－ＮＭＲ核磁共振技术都能准确地测量出烷基多苷的平均聚合度,可判断出烷基多苷中主要苷类的出峰位置。     

Thiazolidine Derivatives as Chiral Catalysts in the Enantioselective Addition of Diethylzinc to Benzaldehyde

Enantioselective addition ofdialkylzinc to aldehydes in the presence of catalytic amountsof chiral catalysts is one of the most important asymmetric C-C bond formation reactions.In most cases chiral fi -amino alcohols or their analogies were used as efficient catalystsin this reactionl.Several chiral catalysts based on the thiazolidine ring have been reported, whichshowed moderate enantioselectivity'. While esters or their derivatives were seldom usedas efficient catalysts. But in our previou…     

三菲咯啉合铁手性配合物键合DNA的立体选择性

应用光谱法研究了手性金属配合物［Ｆｅ（ｐｈｅｎ）３］＾２＋与小牛胸腺ＤＮＡ的作用，确定了△型异构体对Ｂ型右手螺旋ＤＮＡ有优先键合的立体选择性。     

光催化抗雾膜材料的制备及其亲水性研究

采用改进的Ｓｏｌ－Ｇｅｌ技术制备负载型复合光催化抗雾膜材料,ＡＥＳ和接触角测定等手段研究了膜厚度、热处理条件及光照条件等因素对材料亲水性的影响,光催化抗雾膜的亲水性受控于ＴｉＯ２的晶型和膜比表面,大比表面和高锐钛矿含量可降低膜对水的接触角,膜的厚度通过改变催化剂量和光利用率影响材料的亲水性。膜材料亲水性保持或恢复效果相当。     

An interlaboratory capillary zone electrophoresis-UV study of various monoclonal antibodies,instruments, and ε-aminocaproic acid lots

Capillary zone electrophoresis ultraviolet (CZE-UV) has become increasingly popular for the charge heterogeneity determination of mAbs and vaccines. The ε-aminocaproic acid (eACA) CZE-UV method has been used as a rapid platform method. However, in the last years, several issues have been observed, for example, loss in electrophoretic resolution or baseline drifts. Evaluating the role of eACA on the reported issues, various laboratories were requested to provide their routinely used eACA CZE-UV methods, and background electrolyte compositions. Although every laboratory claimed to use the He et al. eACA CZE-UV method, most methods actually deviate from He's. Subsequently, a detailed interlaboratory study was designed wherein two commercially available mAbs (Waters’ Mass Check Standard mAb [pI 7] and NISTmAb [pI 9]) were provided to each laboratory, along with two detailed eACA CZE-UV protocols for a short-end, high-speed, and a long-end, high-resolution method. Ten laboratories participated each using their own instruments, and commodities, showing excellence method performance (relative standard deviations [RSDs] of percent time-corrected main peak areas from 0.2% to 1.9%, and RSDs of migration times from 0.7% to 1.8% [n = 50 per laboratory], analysis times in some cases as short as 2.5 min). This study clarified that eACA is not the main reason for the abovementioned variations.     

First Total Synthesis of (±)-13-Hydroxyneocembrene

First total synthesis of (±)-13-hydroxyneocembrene ( 1 ), starting from 6-methyl-5-hepten-2-one ( 6 ) and geraniol ( 7 ), is described. The key steps are (i) the addition of sulfur-stabilized carbanion 12 to aldehyde 9 , (ii) the synthesis of 18 by using phase-transfer catalyzed coupling reaction, and (iii) low-valent titanium-induced intramolecular coupling of oxo aldehyde 3 to afford the target molecule after the final deprotection.     

Determination of 2,4-D and Dicamba in food crops by MEKC

Summary The determination of 2,4-D (2,4-dichlorophenoxyacetic acid) and Dicamba (2-methoxy-3,6-dichlorobenzoic acid) residues in sugar cane, rice and corn was performed by a supercritical fluid extraction (SFE) method using CO₂/acetone as extraction mix and an SFE apparatus developed in our laboratory. The extracts were cleaned up after extraction by both liquid-liquid partition and a Florisil column. Micellar electrokinetic capillary chromatography (MEKC) coupled with ultraviolet on-column detection was used for the analysis of these pesticides. The detection limits were improved by the preparation of a special detection cell with an increased pathlength that gave detection limits of ca. 0.6 pg for 2,4-D and Dicamba. Our results demonstrated that capillary electrophoresis can be a powerful new analytical tool for pesticide residue analysis.     

BaPbO_3－Nd_2O_3系陶瓷导电性研究

研究了ＢａＰｂＯ３－Ｎｄ２Ｏ３系陶瓷的导电性，研究表明，此系统陶瓷的导电载流子是氧缺位中存在的施主电子；添加适量的Ｎｄ２Ｏ３，可以改善ＢａＰｂＯ３陶瓷的导电性和ＰＴＣ特性