Simultaneous Determination of Baicalin, Baicalein, Wogonin, Oxysophocarpine, Oxymatrine and Matrine in the Chinese Herbal Preparation of Sanwu-Huangqin-Tang by Ion-Paired HPLC

A sensitive and reliable ion-paired high-performance liquid chromatographic method has been established for the simultaneous quantification of six major active ingredients, namely baicalin, baicalein, wogonin, oxysophocarpine, oxymatrine and matrine in the Chinese herbal preparation, Sanwu-Huangqin-Tang. HPLC analyses were performed on a Phenomenex luna C₁₈ column with mobile phase of methanol–acetonitrile–aqueous phosphoric acid at a flow rate of 0.9 mL min⁻¹. The complete separation was achieved within 35 min for the six target constituents. A good linear regression relationship between peak-areas and concentrations was obtained over the range of 12.10–242.0 μg*mL⁻¹ for baicalin, 5.05–101.0 μg*mL⁻¹ for baicalein, 0.95–19.0 μg*mL⁻¹ for wogonin, 2.75–55.0 μg*mL⁻¹ for oxysophocarpin, 2.75–55.0 μg*mL⁻¹ for oxymatrine and 4.90–98.0 μg*mL⁻¹ for matrine, respectively. The repeatability was evaluated by intra- and inter-day assays with relative standard deviation (RSD) being less than 5.1%. The recoveries, measured at three concentration levels, varied from 93.8 to 102.1%. The assay was successfully applied for determination of six bioactive compounds in Sanwu-Huangqin-Tang. The interaction of chemical constituents was observed when the herbs were used in compatibility. The results indicated that the developed assay method was rapid, accurate and could be readily utilized as a quality control method for Sanwu-Huangqin-Tang.     

Ketoreductases: stereoselective catalysts for the facile synthesis of chiral alcohols

The results of a reduction of a wide range of ketones using 31 commercially available isolated ketoreductases (KREDs) are presented. All enzymes accepted a wide substrate range. The stereoselectivity of each enzyme was measured for the reduction of benzoyl-hydroxyacetone and ethyl-3-oxobutanoate, and in each case, enzymes which produce enantiomerically pure (R)- and (S)-alcohols were found. The preparative scale reactions were investigated using two ketones with different hydrophobicities (benzoyl-hydroxyacetone and α-tetralone) and using enzymes with varying specific activities for their reduction. Regardless of the hydrophobicity of the substrate, high titers of ketone (0.75–1.4 M) were reduced in high yield using catalytic amounts of enzyme (1–7% g/g relative to substrate) and cofactor (0.1–0.2% equiv. relative to ketone) within 4–24 h. The cofactor was efficiently regenerated in situ via the oxidation of glucose by glucose dehydrogenase, an enzyme that has also been cloned and over-expressed. These results show that isolated ketoreductases can be quickly and easily screened against target ketones, and the reactions can be scaled to produce preparative amounts of chiral alcohols. Ketoreductase enzymes should become a standard addition to the organic chemists toolbox of asymmetric catalysts for stereoselective ketone reduction.     

单一分散氧化铁-葡聚糖纳米粒子的制备及超顺磁性

0引言 氧化铁-葡聚糖(Fe3O4-Dextran)复合粒子由于具有良好的生物相容性和优异的靶向性能,被用做药物、细胞、酶的载体广泛应用于生物医学、细胞学、生物工程和工业工程等领域[1～3].目前其制备方法主要有一步法和两步法.一步法中氧化铁是在葡聚糖体系下制备的,葡聚糖在氧化铁成核过程中能隔离和分散磁性粒子,防止磁性粒子的团聚和沉积[5].     

SN2 reaction of 2-substituted 3-piperidinol mesylate with retention of configuration: application to the asymmetric synthesis of (2R,3S)-CP-99,994

Starting from protected (S)-3-hydroxyglutarimide 2a, the asymmetric synthesis of (2R,3S)-CP-99,994 8 was achieved. The crucial steps were a neighboring group participation leading to pyrrolidino-aziridinium intermediate 25 and the subsequent regioselective ring-opening reaction. In the case where neighboring group participation was not involved, only the eliminated product 15 was obtained.     

Enantioselective synthesis of epimeric cis-3-carboxycyclopentylglycines

Two epimeric chiral cyclopentylglycines (−)-16 and (+)-17, functionalised with a carboxy group cis to the amino acid group, were prepared starting from chiral 2-amino-3-oxo-norbornanecarboxylic acid derivative exo-9 by combining two classical reactions such as the Diels–Alder and retro-Claisen reactions. Compounds 16 and 17 are non-proteinogenic amino acids of biological interest containing conformational constraints in which the skeletons of both 2-aminoadipic acid and 2-aminopimelic acid are included.     

阻抗谱定量分析金属/有机涂层界面粘接力

采用传输线类型的CR电路解析阻抗谱得到离散的电容参数,它们随离散特征频率变化的线性区间斜率与有机涂层/金属界面的瞬时脱层速率有关,不受缺陷位置腐蚀产物的影响,重现性好.建立了阻抗谱与粘结力的定量关系和数据处理方法,并进行了验证,说明了精度较高的原因.用硅烷直接预处理,或者磷化、热浸锌后再处理,会明显影响A3钢与环氧粉末涂层之间的粘结力.     

Af-AaDd型氢键体系的网络结构参数

利用溶胶-凝胶分配理论对氢键溶液的模型体系进行研究, 给出了凝胶点后氢键网络中各结构参数的计算方案, 并进行相应的数值计算. 结果表明, 因受体基团本身的性质及两类质子受体基团的数量比不同, 受体基团的竞争作用对网络结构有明显影响, 这提供了控制氢键网络结构特征的可能方法.     

Synthesis and in vitro-Anti-hepatitis B Virus Activities of Several Ethyl 5-Hydroxy-lH-indole-3-carboxylates

A series of ethyl 5-hydroxyindole-3-earboxylates 6a-10r was designed and synthesized. The structures of all the compounds were confirmed by IR, ^1H NMR, and MS and their anti-hepatitis B virus （HBV） activities were evaluated in 2.2.15 cells. Among them, compound 7g { ethyl 5-hydroxy-2- [ （ 3-methoxyphenylsulfinyl ） methyl ] -1-methyl-4- [ （4-methylpiperazin-1-yl） methyl ]-1H-indole-3-carboxylate} displays a significant anti-HBV activity, which is more potent than the positive control lamivudine.     

两性喹诺酮抗菌药生理环境下独特的分子荷电性质

本文采用脂质体/水分配系统来考察pH、磷脂的种类和荷电性对药物与有序磷脂膜结合的影响.     

低温水热合成异形TiO2纳米晶及其表征

70 ℃下在钛酸四丁酯(TBOT)水热合成TiO2过程中, 加入油酸, 控制TiO2颗粒的生长方向, 无需热处理, 直接得到针状和纺锤形锐钛矿TiO2纳米晶. 应用透射电子显微镜、X 射线衍射仪对TiO2纳米晶进行了形貌观察和晶体结构的测定. 红外光谱分析表明, 油酸分子以静电作用吸附于针状TiO2纳米晶的表面. 根据UV-Vis吸收峰, 计算了TiO2纳米晶的禁带宽度. 纺锤形TiO2纳米晶具有较高的光催化活性, 60 min内催化降解了90%的罗丹明B.