Determination of gastrodin,p-hydroxybenzyl alcohol, vanillyl alcohol,p-hydroxylbenzaldehyde and vanillin in tall gastrodia tuber by high-performance liquid chromatography

Summary A high-performance liquid chromatographic method for the separation and determination of gastrodin,p-hydroxybenzyl alcohol, vanillyl alcohol,p-hydroxylbenzaldehyde and vanillin in extract of Chinese herbal medicine tall gastrodia tuber (Chinese name: Tianma) was established. The chromatographic conditions were optimized by means of computer-assisted method development technique. Dry-Lab software was used to model the retention behavior of the compounds as a function of gradient conditions, based on the data from two scouting gradient runs. Under the optimized conditions: column, Kromasil-C18, 5 μm, 15×0.46-cm; solvent A, water; solvent B, methanol; gradient, 5/44/65/65% B at 0/9/12/15 min; flow rate, 1.00 mL min⁻¹; temperature, ambient, the quality of tall gastrodia tubers from different sources and tianma injection were examined.     

新的酚型开链冠醚及由其衍生的二苯并冠醚的合成

将水杨醛与碱和氯甲基甲基醚反应, 再经过NaBH4还原, 即制得邻(甲氧基甲氧基)苯甲醇, 然后将其在DMF中与NaH和二(或三)甘醇二对甲苯磺酸酯反应, 得开链冠醚1a和1b。1a和1b经稀酸水解, 即脱保护而分别生成新的酚型开链冠醚2a和2b。用2a与二甘醇二对甲苯磺酸酯和NaH在DMF溶液中反应, 合成顺型二苯并-20-冠-6(3); 而2a与环氧氯丙烷在NaOH水溶液中反应, 则合成了17-羟基二苯并-18-冠-5(4)。     

MoO3—SiO2表面复合物金属催化剂载体的制备与表征

采用ＭｏＯＣｌ４的盐酸溶液负载于ＳｉＯ２的表面反应法，制备了负载型和键联型两种ＭｏＯ３－ＳｉＯ２（ＭｏＳＯ）表面复合物载体。利用红外光谱法研究了ＭｏＳＯ的表面构造及其化学吸附性能；并利用ＴＰＲ技术考察了该表面复合物载体对负载金属Ｐｄ，Ｃｕ氧化物还原过程的影响。     

Synthesis and biological activity of <Emphasis Type="Italic">N</Emphasis>-(2-hydroxyethyl)cytisine derivatives

Derivatives of N-(2-hydroxyethyl)cytisine, N-(2-hydroxypropyl)-, N-(2-hydroxy-2-(1-adamantyl)ethyl)-, and N-(2-hydroxy-2-phenylethyl)cytisine, were synthesized by reduction of N-(2-oxopropyl)-, N-(2-oxo-2-(1-adamantyl)ethyl)-and N-(2-oxo-2-phenylethyl)cytisine with metal hydrides. The antiarrhythmic and analgesic activities of the prepared compounds were investigated. __________ Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 157–162, March–April, 2007.     

Determination of Polyvinyl Alcohol Using Gel Filtration Liquid Chromatography

Gel filtration chromatography using a TSKgel G2000 SW column coupled with differential refractive index detection was used to analyse five grades of polyvinyl alcohol. Limits of detection and quantification for the assay were 0.14 mg mL^–1, 0.47 mg mL^–1 respectively. The inter and intra-day co-efficient of variance were both <7%. There was a significant difference (p<0.05, n=5) between the calibration curves across the five grades of PVA due to a refractive index range of 13.0790 –1.3181 (n=3). The assay accuracy was 98.99% ± 8.97% (n=5) and 90.60% ± 7.87% (n=5) of a spiked PVA sample was recovered from a commercial formulation.     

Ag／Al2O3选择性催化丙烯还原氮氧化物表面反应机理的原位红外光谱研究

 在富氧条件下Ag／Al2O3对以丙烯为还原剂选择性催化还原NOx的反应有很高的催化活性．本实验成功地利用原位红外光谱分析手段,在真实的催化反应条件下,探讨了丙烯选择性还原NOx的反应机理,证实了催化剂表面反应中间体Al－NCO和Ag－NCO虽在真空中稳定,但在实际反应条件下极为活泼．催化剂表面上R－ONO和R－NO2分解成NCO是整个反应的速度控制步骤．这一结论与在真空系统条件下对其反应机理的研究结果一致,证明了在这一反应体系中两种研究方法的相关性．同时本实验还从反应机理上探讨了催化剂的水蒸气中毒现象．水蒸气的存在阻碍了催化剂表面R－ONO和R－NO2的生成,并进一步阻碍了反应的速度控 制步骤,即R－ONO和R－NO2向Al－NCO和Ag－NCO的转化,但这是一种完全可逆的暂时中毒现象．结合相应的催化剂活性评价结果对表面反应机理进行了讨论．     

钙的加入对含锆熔铁型氨合成催化剂性能的影响

近年来，对于熔铁型氨合成催化剂在不断通过加入新的助剂来改善其性能。本文用Mossbauer谱等手段分析与研究加入钙后对含锆催化剂的影响。     

介体型乙醇生物传感器的研制及应用

本文报道了电流型乙醇生物传感器的研制与应用。该传感器以健合型耐尔蓝修饰浸蜡石墨电极为基体电极，将乙醇脱氢酶及ＮＡＤ＾＋固定在人造丝网上，成为一种无试剂的乙醇生物传感器。在ｐＨ８．８的Ｔｒｉｓ／ＨＣｌ介质中，该传感器的响应电流与乙醇浓度在０．１０－１．０ｍｍｏｌ／ｌ范围内有良好的线性关系。     

辅酶NAD(P)H模型分子的研究进展

辅酶NAD(P)H在生物体内起着重要的调节作用, 已引起了有机化学工作者极大的兴趣, 尤其是在还原反应的立体选择性上, 人们已经开展了大量的研究工作. 讨论了NAD(P)H模型分子进行立体专一性还原反应的影响因素, 并对NAD(P)H模型分子的研究工作做了总结.     

Synthesis and Crystal Structure of (2S,2'S,4'R)-2-(1-Hydroxy-1-ethylpropyl)-1-[(1'-p-tosyl-4'-hydroxypyrrolidin-2'-yl)methyl]pyrrolidine

1 INTRODUCTION In recent years, chiral β-amino alcohols have attracted much attention due to their special bio- logical functions and catalytic activities. Chiral β- amino alcohol moieties are usually found not only in natural products (e.g., cinchona alkaloids, ephe- drine, toxal, etc.) with special biological activities[1, 2], but also critical structural segments of some syn- thesized biologically active compounds, such as adrenergic agonists or antagolist[3, 4] and inhibitors for HI…