基于中空纤维液相微萃取的麻黄碱和伪麻黄碱优势构象的确定及含量测定

利用中空纤维液相微萃取方法(HF-LPME)分析麻黄碱和伪麻黄碱在不同基质中的优势构象,阐明了麻黄碱和伪麻黄碱的萃取机理;结合高效液相色谱(HPLC)建立了微量麻黄碱和伪麻黄碱的分离测定方法。以聚偏氟乙烯中空纤维为有机溶剂载体,正己醇为萃取溶剂,麻黄碱和伪麻黄碱的NaOH(5 mol/L)溶液为样品相,0.01 mol/L H2SO4溶液为接收相,在1200 r/min转速下萃取35 min,收集萃取液直接进行HPLC分析。麻黄碱和伪麻黄碱在水溶液中的线性范围为5～100 μg/L,检出限分别为1.9 μg/L和1.2 μg/L,富集倍数分别为38和61倍,平均回收率分别为100.6%±1.2%和103.2%±3.5%;在鼠尿液中的线性范围为100～5×104 μg/L,检出限分别为30 μg/L和42 μg/L,富集倍数分别为20和17倍,平均回收率分别为108.4%±4.4%和106.1%±5.4%。研究表明该方法操作简单,选择性高,适用于微量麻黄碱的含量测定和分析。     

长喙毛茛泽泻的胚胎发生

对长喙毛茛泽泻（Ｒａｎａｌｉｓｍａｒｏｓｔｒａｔｕｍ）胚及胚乳的发育进行了研究．合子横向分裂成基细胞和顶细胞，基细胞不再分裂，顶细胞分裂形成胚体及合点端胚柄细胞．胚发育属石竹型．成熟胚为“Ｕ”形．胚乳发育属沼生目型，初生胚乳核在近合点端横向分裂，形成两个不等室，即合点室和珠孔室．合点室细胞不再分裂，珠孔室细胞经游离核分裂后，从珠孔端及合点端同时开始细胞化．细胞化与成膜体、细胞板有关，而不是通过“自由生长壁”．随着胚的发育，胚乳逐渐解体，成熟种子中无胚乳．在原胚发育时期，胚柄基细胞及合点室胚乳细胞体积增大，核染色深，有时分裂成２～３核，细胞质浓厚．它们在四形胚时期开始退化，与胚乳细胞化相对应，推测它们与胚早期发育所需营养的供应有关．     

树脂法分离纯化倒提壶生物碱的研究

采用阳离子交换树脂和大孔吸附树脂联用的方法,将倒提壶生物碱提取液依次经过阳离子交换树脂和两次大孔吸附树脂,对其中的天芥菜碱和毛果天芥菜碱进行分离纯化。结果表明,倒提壶生物碱溶液采用阳离子交换树脂经过水洗和NaCl洗脱与大孔吸附树脂两次经乙醚和50%乙醇洗脱后,毛果天芥菜碱与天芥菜碱的纯度分别从0.73%和2.2%提高至81.6%和79.2%,提取量分别由4.6 mg/g和10.7 mg/g提高至50.6mg/g和92.7 mg/g。该文所建立的分离纯化方法具有成本低、污染小、周期短、操作简便和分离纯化效率高等特点,适合工业化生产。     

Supercritical fluid extraction ofCymbopogon citratus (DC.) Stapf

Summary Cymbopogon citratus (DC.) Stapf. is also known as lemon grass; its leaves produce a volatile oil upon steam extraction which is used for medicinal purposes. This work describes the supercritical fluid extraction ofCymbopogon citratus in sequential and dynamic extraction modes. Different modifiers for supercritical carbon dioxide were used for the extractions. Principal compounds in the essential oils were analyzed by GC and GC-MS and identified as neral, geraniol, geranial, nerolic acid and geranic acid. Different chromatographic profiles were obtained when the type and proportion of modifier were changed.     

长喙毛茛泽泻的大小孢子发生及雌雄配子体发育

长喙毛茛泽泻（ＲａｎａｌｉｓｍａｒｏｓｔｒａｔｕｍＳｔａｐｆ）花药壁的发育属单子叶型，绒毡层为周原质团型．花粉母细胞减数分裂时的胞质分裂为连续型，四分体呈左右对称式排列，个别为交工型．成熟花粉为３细胞型，双珠被，薄珠心，倒生胚珠．大孢子母细胞由孢原细胞直接发育而来，成熟胚囊为８核组成的７细胞胚囊，两个极核在受精前不融合成次生核     

长喙毛莨泽泻双受精过程的细胞学观察

对长喙毛莨泽泻双受精过程进行了细胞学观察，结果表明，开花前３ｈ已可观察到花粉管进入胚囊，开花前２ｈ至开花后８ｈ，大部分雌、雄性核发生融合．合子内的雌、雄性核仁可以融合，以一个大核仁的形式进入分裂期，但核仁正在融合或尚未开始融合的合子同样可以进入分裂期．初生胚乳核内的核仁存在３种情况，即３个核仁或者不融合，或者精子核仁与珠孔端极核核仁融合，或者３个核仁融合成一个大核仁．配子融合属于有丝分裂前的配子融合类型．同一朵花中不同心皮的受精过程有一定顺序，即自花托下部逐渐向上部完成受精作用．     

Separation of four flavonol glycosides from Solanum rostratum Dunal using aqueous two‐phase flotation followed by preparative high‐performance liquid chromatography

Aqueous two‐phase flotation followed by preparative high‐performance liquid chromatography was used to separate four flavonol glycosides from Solanum rostratum Dunal. In the aqueous two‐phase flotation section, the effects of sublation solvent, solution pH, (NH₄)₂SO₄ concentration in aqueous solution, cosolvent, N₂ flow rate, flotation time, and volumes of the polyethylene glycol phase on the recovery were investigated in detail, and the optimal conditions were selected: 50 wt% polyethylene glycol 1000 ethanol solvent as the flotation solvent, pH 4, 350 g/L of (NH₄)₂SO₄ concentration in aqueous phase, 40 mL/min of N₂ flow rate, 30 min of flotation time, 10.0 mL of flotation solvent volume, and two times. After aqueous two‐phase flotation concentration, the flotation products were purified by preparative high‐performance liquid chromatography. The purities of the final products A and B were 98.1 and 99.0%. Product B was the mixture of three compounds based on the analysis of high‐performance liquid chromatography at the temperature of 10°C, while product A was hyperoside after the identification by nuclear magnetic resonance. Astragalin, 3’‐O‐methylquercetin 3‐O‐β‐d ‐galactopyranoside, and 3’‐O‐methylquercetin 3‐O‐β‐d ‐glucopyranoside were obtained with the purity of 93.8, 97.1, and 99.2%, respectively, after the further separation of product B using preparative high‐performance liquid chromatography.     

Two new triterpenoid saponins obtained by microbial hydrolysis with Alternaria alternata AS 3.6872

Compound 1, a triterpenoid saponin from Ardisia gigantifolia Stapf showing potential anti-tumour activity, was hydrolysed into two deglycosyl derivatives (2 and 3) by Alternaria alternata AS 3.6872. Both these derivatives are new compounds. Their structures were elucidated on the basis of 1D, 2D NMR, HR-ESI-MS and optical rotation spectral data. Compounds 1–3 were evaluated for their cytotoxicity against human hepatocellular carcinoma and normal liver cells by Cell Counting Kit 8 colorimetric assay.     

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。