鸡骨草和相思子中相思子碱的反相高效液相色谱分离和测定

用反相高效液相色谱分离并测定定了鸡骨草和相思子中的相思子碱，建立了中药中相思子碱分离、测定的色谱法。     

密闭微波辅助提取-HPLC法测定还亮草中硬飞燕草碱和巴比翠雀碱的含量

采用密闭微波辅助法(PMAE)提取还亮草中的硬飞燕草碱和巴比翠雀碱。采用单因素试验结合正交试验方法对微波实验条件进行优化。得到硬飞燕草碱和巴比翠雀碱的最佳提取方案:药物颗粒度100目,固液比1∶60,微波温度80℃,微波功率560 W,微波时间10 min。以甲醇-0.2%三乙胺(45∶55)为流动相,建立了高效液相色谱(HPLC)测定硬飞燕草碱和巴比翠雀碱含量的方法。硬飞燕草碱和巴比翠雀碱分别在0.50~50.0,0.30~30.0 mg/L范围内呈良好的线性关系,回收率为98.3%~104.5%,相对标准偏差(RSD)分别为2.0%和2.2%。与传统溶剂回流法(SRE)进行比较,该方法简单、提取率更高。     

聚焦微波辅助提取/HPLC法测定倒提壶中天芥菜碱的含量

采用正交实验方法对聚焦微波辅助提取(FMAE)的实验条件进行优化,以天芥菜碱为提取目标物,HPLC法测定其含量。通过优化,得到最佳实验条件:药材粒度60目,液料比1∶35,微波功率420 W,微波时间50 min。HPLC分析条件:以甲醇-0.05%三乙胺(pH7.5)(30∶70)为流动相,在220 nm处检测,天芥菜碱的线性范围为52~1 040 mg/L,相关系数(r)为0.999 9,检出限为0.040 2 mg/L,其加标回收率为97.5%~103%,相对标准偏差为2.4%,方法简单、灵敏度高。     

微波辐射-溶剂回流法提取/HPLC法测定倒提壶中天芥菜碱与毛果天芥菜碱的含量

采用单因素试验,对微波辐射-溶剂回流提取法的实验条件进行优化,得到最佳提取条件:药材颗粒度100目,微波功率60%档(总功率为700 W),微波辐射时间90 s,固液比1∶25,提取温度90℃,提取时间45 min。以天芥菜碱和毛果天芥菜碱为提取目标物,通过HPLC法测定其含量,其分析条件为:以乙腈-0.1%乙酸溶液(p H 5.6,体积比5∶95)为流动相,在220 nm处检测。毛果天芥菜碱和天芥菜碱的浓度在50~900 mg/L范围内均呈良好线性关系,检出限分别为1.50 mg/L和1.52 mg/L,加标回收率分别为95.0%~98.5%和96.5%~101%,RSD分别为1.8%和2.4%,方法简单、灵敏度高。     

长柱十大功劳中药根碱、巴马汀和小檗碱的高效液相色谱法同时测定

建立了高效液相色谱法同时测定长柱十大功劳中药根碱、巴马汀、小檗碱含量的方法.样品用盐酸-甲醇(体积比1:100)混合溶液超声提取,C18柱色谱分离,以乙腈-0.05 mol/L磷酸二氢钾缓冲液(磷酸调Ph值至3.0)(体积比28:72)为流动相,检测波长:265 nm.方法线性良好,相关系数均大于0.999,盐酸药根碱、盐酸巴马汀、盐酸小檗碱的加标回收率及相对标准偏差分别为99%,1.43%; 100%,1.93%; 99%,2.82%.     

光度法测定槟榔中槟榔碱的含量

采用柱色谱法从槟榔中提取分离槟榔碱,用红外(1R)、核磁(HNMR)、质谱(MS)法确证其结构。采用溴甲酚绿光度法测定槟榔碱的含量,线性回归方程为A=7.160×10~(-3)c-0.0328,相关系数r=0.9954,线性范围为19.5～112.1μg/ml。对样品进行测定,相对标准偏差为0.556％,回收率为96.9％～102.8％。     

微波间歇萃取-分光光度法测定三七中总皂苷

本文建立了采用微波辅助间歇提取三七样品中的总皂苷,并以分光光度法测定其含量的实验方法。分别通过单因素实验和正交实验设计,优化了萃取溶剂浓度、溶剂用量、微波功率和微波辐射时间等提取条件,确定了微波辅助萃取法提取三七中皂苷类化合物的最佳条件为:使用浓度为60%的乙醇,在液固比100∶1的条件下,以255 W的微波功率,微波间歇萃取10×20 s。在上述最优条件下进行了精密度和回收率实验,加入回收率在97.7%~101.8%之间,RSD为1.54%(n=5)。与传统的索氏提取法和超声波提取法比较,微波辅助萃取法具有操作简便,宽速,重现性好等特点,实验结果表明此方法可推广应用于各类中草药中总皂苷的含量测定。     

微波辅助提取-可见分光光度法测定穿心莲中的总黄酮

比较了微波辅助提取、超声提取、索氏提取3种方式对穿心莲中总黄酮的提取效率.确定以微波辅助提取法最佳.实验结果表明:用60%乙醇在固液比为1:15的条件下提取6 min提取效率最高.用NaNO2-硝酸铝-NaOH-黄酮体系分光光度法测定总黄酮含量,平均回收率为103.00%,RSD=1.37%(n=5),证实了可以用微波辅助提取法提取,紫外可见分光光度法检测穿心莲中总黄酮的可行性.     

吴茱萸中吴茱萸次碱与吴茱萸碱含量的超临界流体色谱法测定

建立了超临界流体色谱法分离测定吴茱萸中吴茱萸次碱和吴茱萸碱含量的方法,并研究了其影响因素。使用Kromasil Slica填充柱,流动相为含13%甲醇的CO2,流速2.0 mL.min-1,柱温60℃,背压2.0×107Pa,检测波长225 nm,测得吴茱萸次碱和吴茱萸碱的线性范围分别为0.33~8.25μg(r=0.999 3)、0.68~17μg(r=0.999 8),平均加标回收率均为100%。与传统方法相比,超临界流体色谱可在简单的流动相条件下对吴茱萸中的吴茱萸次碱和吴茱萸碱进行良好分离。     

萝芙木根中萝芙木碱的分离纯化

对萝芙木根中萝芙木碱的提纯与检测技术进行研究.利用萝芙木植物的根和皮为原料,对萝芙木碱的分离纯化过程进行了系统的研究,确立了固一液萃取、液一液萃取、等电点沉淀、甲醇重结晶提取萝芙木碱的优化方案,并用高效液相色谱法检测了萝芙木碱的含量.实验所得样品中萝芙木碱的含量不低于98%.结果表明该分离纯化技术生产成本低,操作简单,...     

多环芳二酐型聚酯亚胺膜的透气性能

多环芳二酐型聚酯亚胺膜的透气性能李悦生，丁孟贤，徐纪平（浙江大学高分子科学与工程研究所，杭州，３１００２７）（中国科学院长春应用化学研究所）关键词聚醚酰亚胺，聚酯酰亚胺，膜，透气性通常的聚酰亚胺加工性能较差，在芳环二酐的苯环间引入醚键等柔性基团后，其...     

Determination and study on residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil

A QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for the determination of benazolin-ethyl and quizalofop-p-ethyl in rape and soil by high-performance liquid chromatography-tandem mass spectrometry has been developed in this study. The residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil were determined with the developed method. The half-lives of benazolin-ethyl in rape straw and soil were 3.7–5.1 days and 14.3–26.3 days, respectively. The half-lives of quizalofop-p-ethyl in rape straw and soil were 5.0-6.1 days and 0.3–9.7 days, respectively. The residue of benazolin-ethyl and quizalofop-p-ethyl in rapeseed and soil were below the detection limit (i.e., 0.5?mg?kg^?1, the maximum residue level of European Union for quizalofop-p-ethyl).     

微量元素与疾病诊断治疗的研究现状及展望

对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述，包括：微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。     

Ferrocene and ferrocenium modified clays and their styrene and EVA composites

In this work, ferrocene- and ferrocenium-containing salts were employed to modify montmorillonite. X-ray measurements show an increase in the interlayer spacing upon clay modification, which means that the larger and more organophilic cations were inserted into the gallery space of montmorillonite. Attempts to prepare nanocomposites of polystyrene and ethylene vinyl acetate copolymers lead to immiscible systems; the morphology of these systems was elucidated with TEM, XRD and cone calorimetry. The thermal stability of the composites is greater than that of the virgin polymer.     

Ti-V基储氢合金及其氢化物的物相结构与组分优化设计

Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB₅型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。     

钒与糖代谢及糖尿病

微量元素钒作为生物体内必需元素，经证实有很重要的生理学功能，与机体糖代谢有十分密切的关系，且能降低糖尿病动物模型的高血糖，极有可能被开发为治疗糖尿病的药物。     

Synthesis and Optical and Redox Properties of Symmetric and Asymmetric BODIPYs

Herein, we present the synthetic route and the photophysical, electrochemical as well as laser properties of novel red‐emitting boron‐dipyrromethenes (BODIPYs) bearing arylethyne moieties. Such functionality is added along the main axis of the chromophore leading to single‐ and double‐substituted derivatives. The relationship between the dye structure and the lasing properties is studied in detail with the help of the photophysical and electrochemical properties as well as quantum mechanical simulations. The asymmetric substitution of the parent dye induces inhomogeneities in the charge distribution, which leads to an overall loss of the fluorescence capacity, mainly in polar media. Such non‐radiative deactivation processes can be softened by decreasing the electron‐donor ability of the substituent or even avoided by symmetrical substitution. Thus, grafting of the arylethyne moieties at the longitudinal axis of the indacene core results in an effective strategy to develop red‐edge BODIPYs with highly efficient and photostable laser emission.     

Conformations and steric and stacking interactions of trisubstituted ureas and thioureas with alkyl and phenyl groups

The monomeric ν(N—H) vibrations of various trisubstituted ureas of the R₂UPh type and -thioureas of the R₂TUPh type have been studied. The trans—out isomerism in the former and the trans—out—cis isomerism in the latter are discussed from the point of view of steric effect. The monomeric ν(N—H) vibrations of RPhUPh and RPhTUPh are also examined. The single band appearing in the spectrum of both ureas is characteristic of the cis form; this suggests the existence of phenyl—phenyl interaction (the stacking interaction proposed by Galabov et al. [10]). Behavior of ν(N—H) vibrations at several concentrations is shown to be clearly different in the three forms (trans, out and cis). The presence of the cis form is confirmed by solvent effect experiments.     

含茂基苯并三氮唑基镧系有机配合物的合成及表征

三茂基镧系化合物和苯并三氮唑在四氢呋喃中反应,合成了7个未见文献报道的含茂基苯并三氮唑基镧系有机配合物,经元素分析、IR和MS测定,从有关数据推测了这类配合物的可能结构。