高分辨电感耦合等离子质谱测定黄连中的微量元素

文章采用高分辨电感耦合等离子体质谱(HR-ICP-MS)的方法,测定了中草药中四种黄连——味连、雅连、马尾连和胡黄连中的微量元素。结果表明:在所有16种稀土元素中,La,Ce,Nd,Gd,Sm,Sc含量较高,胡黄连的稀土总量为5.18μg·g~(-1),是所有四种黄连的最高者,其次是雅连和马尾连,最低的是味连(1.26μg·g~(-1))。而对于与清热解毒有关的金属无素如Mg,Mn,Zn,Ca和Fe元素,雅连中Mg,Mn,Zn的含量最高。高Fe和Ca的含量存在于马尾连和胡连之中。在测定不同提取方法的提取物中发现,只有部分的稀土元素能被醇和水所提取,它们分别是31.6％和4.1％。清热解毒元素的提取率明显高于稀土元素。     

目标因子分光光度法同时测定中成药复方五味子中三项活性成分

将目标因子分光光度法应用于五味子提取液中五味子甲素、五味子乙素、五味子醇甲等三项活性成分的同时测定,介绍了基本原理和具体的分析步骤,运用计算机VC 语言对试验数据进行回归分析。试验结果表明,目标因子分光光度法对样品各组分的平均回收率在98.9%-106.7%之间,样品不经分离即可同时测定。     

紫荆花红色素开发利用的研究

首次报道紫荆花红色素的提取纯化方法及红色素的理化性质，并与玫瑰茄红色素作对比研究，证实同属于花青甙类化合物，又经急性毒性试验证明其毒性极低，故紫荆花天然红色素具有开发利用的价值。     

毛细管电泳法研究提取剂对黄连-黄柏共煎剂中生物碱含量的影响

用毛细管电泳法,对黄连与黄柏配伍后共煎剂中的主要生物碱进行了分析。以50 mmol/L Na2B4O7(pH=7)-CH3OH(85:15,V/V)为背景电解质,操作电压为14 kV,电迁移进样10 kV×5s,柱上223 nm检测,5种主要生物碱9 min内可在50 cm×75μm毛细管上实现基线分离。以小檗碱、巴马汀的提取量为指标,分析了提取剂对提取效果的影响。以30％的乙醇水溶液为提取剂,可得到最大煎出量。     

毛细管电泳法测定五味子中五味子甲素

采用毛细管电泳法,以15 mmol·L-1磷酸氢二钠、15 mmol·L-1硼砂和20%乙醇的缓冲溶液作为运行电解质溶液,获得了五味子甲素与五味子中其余成分的有效分离,且峰形较好.测得五味子甲素线性回归方程为y=-0.72+24.9 x,相关系数为0.998;线性范围为0.03～0.37 g·L-1.测得的五味子中五味子甲素质量分数为1.18%,相对标准偏差为2.63%(n=6);平均回收率为99.6%.     

微波-同时蒸馏萃取分离肉桂挥发性成分分析

经粉碎的肉桂干燥树皮置于去离子水中微波加热处理后,用自制的同时蒸馏-萃取装置,以重蒸乙醚为溶剂将试样中的挥发组分萃取分离。用旋转蒸发器除去乙醚后即得到含有试样中挥发组分的透明的黄色液体,收得率为6.5%,应用GC/MS法对黄色液体的组分进行定性和定量分析。借助于联机的计算机和相关软件并用峰面积-归一化计算测得其中共有27个化合物,其中含量最高的是肉桂醛,达94.36%。另取部分上述挥发油(即黄色液体),用加成分解法将其中肉桂醛转化为一种加成产物以沉淀形式析出,即将黄色液体与NaHSO3共置于微波炉中,在不超过10℃的条件下处理直至加成物完全析出。将此加成物分出,并用0.1 mol.L-1盐酸进行水解处理,使加成物恢复成纯度较高的肉桂醛,用IR及MS对其组成及结构作进一步确认。     

一种用于中药纯化过程的近红外光谱分析新方法

针对中药大孔吸附树脂纯化过程缺乏在线检测分析手段等问题，提出基于光纤 近红外透射光谱的过程分析新方法．以黄连提取物为例，采用HPLC分析测定值作参 比，用偏最小二乘算法建立了近红外透射光谱校正模型，并成功地用于预测黄连生 物碱在大孔树脂纯化过程中的洗脱曲线．本方法实时、快速，可同时测定洗脱物中 盐酸小檗碱、盐酸巴马亭、盐酸药相碱和黄连总生物碱的浓度．预测精度满足工业 过程分析要求，为提高中药质量分析水平提供了新的途径．     

Furostanol saponins with inhibitory action against COX-2 production from Tupistra chinensis rhizomes

Two furostanol saponins were obtained from the n-butanol fraction of methanol extract from Tupistra chinensis rhizomes,a folk medicine of Shennongjia Forest District of Hubei Province.Their structures were determined as (25S)-26-O-(β-D-glucopyranosyl)- furost-1β,3β,22α,26-tetrol-3-O-β-D-glucopyranosyl-(1→4)-β-D-glucopyranosyl-(1→2)-β-D-glucopyranoside (1) and (25R)- 26-O-(β-D-glucopyranosyl)-furost-1β,3β22α,26-tetrol 3-O-β-D-glucopyranosyl-(1→4)-β-D-glucopyranosyl-(1→2)-β-D-glu- copyranoside (2),on basis of chemical and spectroscopic evidences.1 and 2 displayed marked inhibitory action towards COX-2 production in macrophages of the rat abdomen induced by LPS at 20μg/mL.     

Tupisteroide A–C,three new polyhydroxylated steroidal constituents from the roots of Tupistra chinensis

Three new steroidal compounds with polyhydroxy groups, tupisteroide A–C (1–3), were obtained from the roots of Tupistra chinensis, together with one known compound (4) that was isolated from this plant for the first time. The structures of tupisteroide A–C were determined on the basis of one‐ and two‐dimensional NMR spectroscopy, including ¹H–¹H Correlation Spectroscopy, Heteronuclear Multiple Bond Correlation, and Heteronuclear Single Quantum Coherence experiments. The isolated compounds were evaluated for their cytotoxic activities against A549, HepG2, and CaSki cancer cell lines in vitro. Among them, compounds 1, 2, and 4 did not show significant inhibitory activity, but compound 3 showed cytotoxicity against A549 cancer cell lines with IC₅₀ values of 25.0 μM. Copyright © 2012 John Wiley & Sons, Ltd.     

Ion pair assisted micro matrix solid phase dispersion extraction of alkaloids from medical plant

A novel micro matrix solid phase dispersion method was successfully used for the extraction of quaternary alkaloids in Phellodendri chinensis cortex. The elution of target compounds was accomplished with sodium hexanesulfonate as the eluent solvent. A neutral ion pair was formed between ion-pairing reagent and positively charged alkaloids in this process, which was beneficial for selectively extraction of polar alkaloids. Several parameters were optimized and the optimal conditions were listed as follows: silica gel as the sorbent, silica to sample mass ratio of 1:1, the grinding time of 1 min. The exhaustive elution of targets was achieved by 200 µL methanol/water (9:1) containing 150 mM sodium hexane sulfonate at pH 4.5. The method validation covered linearity, recovery, precision of intraday and interday, limits of detection, limits of quantitation, and repeatability. This established method was rapid, simple, environmentally friendly, and highly sensitive.