脂肪酸酯水解行为及与低聚果糖缔合行为的研究和应用

酯类化合物是酒类产品的主要香味成分,也是化妆品、饮料、食品中主要呈香物质,故对其水解行为的研究对揭示影响酯水解反应因素及提高和稳定上述产品质量,特别是解决酒类产品低度化过程中存在的质量下降问题具有重要的意义[1]。对酯水解反应的研究前人作了大量的工作:Bender与Ma     

Syntheses of Two Potential Ligands for Tc-99m Labeling as Diagnosis Agents of Alzheimer''''s Disease

Two types of ligands-biphenyl and stilbene derivatives, whichcan be labeled with Tc-99m for the diagnosis of Alzheimer'sdisease (AD) have been synthesized successfully. The key stepsin these two syntheses involved Suzuki reaction and Wittig reac-tion respectively. The new discovered debromination reactionmay be expanded to the compounds with double or triple bondadjacent to the carbon atom bearing the bromine atoms. Thesetypes of syntheses provide a route to a series of biphenyl andstilbene derivatives that will benefit the search of new imagingagents for AD.     

尿素法合成高结晶度类水滑石

尿素的高温分解特性被用于控制层状化合物合成过程中的pH值。室温下尿素可与硝酸盐形成均一溶液，当其高温分解时可以保证溶液内部各点的pH值始终一致，因而可获得高结晶度的水滑石样品。利用该法可合成出Mg-Al、Zn-Al及Ni-Al类水滑石，但难以合成出Co-Al，Mn-Al及Co-Cr类水滑石，相信这与不同金属离子发生沉淀时所需的pH值有关。     

Development of an indirect competitive ELISA for the determination of papaverine

Papaverine (1-(3,4-dimethoxybenzyl)-6,7-dimethoxyisoquinoline, PAP) is a member of the benzylisoquinoline sub-group of the opium alkaloids. It has been widely used for treating diseases like pulmonary arterial embolism and renal or biliary colic. In this paper, a specific conjugate of mono-demethylated papaverine-O-carboxylmethyl ether (MDMPAP-O-CME) and bovine serum albumin (BSA) was synthesized and used as the complete antigen (PAP-BSA), with which we successfully obtained a high-titer anti-PAP polyclonal antibody (pAb) by immunization of rabbits. The anti-PAP pAb showed high affinity to papaverine with an affinity constant (K_aff) of 7.3 × 10⁷ L/mol. With this antibody, we established a sensitive immunochemical method for the determination of papaverine based on indirect competitive enzyme-linked immunosorbent assay (ELISA). The optimal concentrations of the coated antigen (PAP-OVA) and purified pAb used in the ELISA were 5 and 1.2 μg/mL, respectively. The cross reactivity of other benzylisoquinoline derived substances, including 1-(3,4-dihydroxybenzyl)-7-hydroxy-6-methoxy-isoquinoline (6-methoxy-papaveroline, MPAPO), morphine (MP) and codeine (CD) were all lower than 1%. The linear range of the calibration curve was 0.1-1000 ng/mL. Normal human serum samples were spiked with known amount of papaverine and measured by the ELISA. Recoveries were between 102% and 105%. Papaverine content in a commercial papaverine hydrochloride injection sample was also determined using the established ELISA. Compared with the results given by the control experiment of HPLC, the recoveries of ELISA to detect injection samples were 102-110%. The limits of detection for synthetic serum samples and injection samples of papaverine hydrochloride were 0.25 and 0.06 ng/mL, respectively.     

Mechanism of α-acetyl-γ-butyrolactone synthesis

The mechanism of α-acetyl-γ-butyrolactone (ABL) synthesis from γ-butyrolactone (GBL) and ethyl acetate (EtOAc) was explored by detecting the material changes involved and the enthalpies of formation of the synthons, products, and possible intermediates were calculated using the density functional theory. GBL forms a carbanion of γ-butyrolactone by losing an α-H under strongly alkaline conditions. ABL is then obtained via two reaction mechanisms. One of the reaction mechanisms involves direct reaction of the carbanion of GBL with EtOAc to produce ABL. The other involves the formation of a carbanion of α-(2-hydroxy-tetrahydrofuran-2-yl)-γ-butyrolactone through the reaction of two molecules of GBL, and the subsequent combination of this anion with EtOAc to produce ABL. ABL is thus formed through the above two kinds of competitive ester condensation reactions. It is unnecessary to take into account synthons’ local thickness, and their self-condensation under these conditions. Both reactions of the carbanion of GBL with EtOAc and GBL are exothermic, so the control of their reaction rate is the key to their security. Considering the reasons above, this work applied synthon as the solvent, and avoided environmental pollution by alkylbenzene; also, accidents such as red material and fire were avoided by specific surface area of sodium metal control. Effective isolation of the organic and aqueous phases was performed using the salting out method. Thus, an environmentally friendly, safe, simple, and efficient new method for the synthesis of ABL with the yield higher than 90 % has been established.     

同位镀铋膜电极测定爆米花中的痕量铅

采用同位镀铋膜法修饰铂电极,用差分脉冲溶出伏安法对爆米花中痕置铅进行了测定,并优化了实验条件.在优化的实验条件下,分别对2.0×10<'8>-6.0×10<'-7>mol/L和6.0×10<'-7>-1.0×10<'-4>mol/L的pb<'2+>进行了测定,Pb<'2+>溶出峰电流与Pb<'2+>浓度呈良好的线性关系...     

Improvement of the performance of an immunoaffinity extraction method via region-specific immobilization of IgG

Using papaverine as a model target, an immunoaffinity column of high selectivity and binding capacity was prepared by utilizing covalent linkage between the Fc portion of IgG and the surface of Sepharose 4B support. Compared with the commonly used random coupling method, the binding capacity of the region-specific immobilized antibodies was increased from 0.04 to 0.2 mol of antigens/mol of antibodies and a much larger concentration factor was thus achieved. The obtained immunoaffinity column has been successfully used in pretreatment of pericarpium papaveris samples. The method offers an improved approach to immunoaffinity extraction that should be useful for purification and concentration of other targeted compounds in highly complex mixture.     

合成方法对MCM-22分子筛的结构、性质及催化性能的影响

在水热条件下分别以动态法和静态法合成了高纯度和高结晶度的MCM-22分子筛.采用N2吸附、XRD、TEM和FTIR等方法研究了制备方法对分子筛的结构及性质的影响.结果表明,动态法合成的MCM-22比静态法合成的分子筛的晶粒小,酸量低.在丙酮一步法合成甲基异丁基酮反应中,静态条件下合成的MCM-22为载体的催化剂的丙酮转化率较高,这是由于该分子筛的酸量较高所致.而MIBK的选择性则呈相反趋势,这可能与动态条件下合成的分子筛粒径小、孔道短有关.     

A new competitive enzyme-linked immunosorbent assay (ELISA) for determination of estrogenic bisphenols

Bisphenol A and other hydroxylated diphenylalkanes (generally known as bisphenols) have been identified as potential estrogenic substances. In this paper, a specific polyclonal antibody was produced against these compounds by immunization of rabbits with a conjugate of 4,4-bis (4-hydroxyphenyl) valeric acid and bovine serum albumin (BHPVA-BSA). The polyclonal antibody showed specific recognition of the bisphenol structure, while the cross reactions of other common phenolic compounds such as phenol, hydroquinol and p-hydroxybenzoic acid were all lower than 1%. The linear range of bisphenol A calibration curve was 1–10 000 ng ml⁻¹. Real water samples and mouse serum samples were spiked with known amount of bisphenol A and measured by the competitive ELISA. Recoveries were between 92 and 105%. The detection limits were found to be 0.1 ng ml⁻¹ for real water samples and 2 ng ml⁻¹ for serum samples. The method is very useful for monitoring bisphenol compounds in environmental and biological samples.     

胺类化合物的离子性指数、极化效应指数与其13C NMR谱化学位移关系

胺类化合物的离子性指数、极化效应指数与其13C NMR谱化学位移关系;脂肪胺化合物;13C NMR谱化学位移;离子性指数;极化效应指数;立体效应