柱前衍生高效液相色谱法测定甘草中甘草酸含量

建立了柱前衍生高效液相色谱测定甘草中甘草酸的新方法。以对硝基溴化苄为柱前衍生化试剂,采用Phenomenex C18分离,以乙腈-3%冰乙酸溶液(体积比60∶40)为流动相,紫外290nm检测。结果表明,在10.0～100.0μg/mL浓度范围内,甘草酸衍生物的峰面积与甘草酸浓度呈现良好的线性关系,相关系数为0.9951,相对标准偏差为2.1%(c=30.0μg/mL,n=6),检出限为1.0μg/mL,加标回收率为96.7%～101.1%。该法准确,灵敏度高,已用于甘草中甘草酸含量的测定。     

同时蒸馏萃取GC-MS分析刺异叶花椒叶挥发油化学成分

研究黔产刺异叶花椒叶挥发油的化学成分，采用同时蒸馏萃取提取并用气相色谱-质谱进行分离测定，共分离出67种成分，鉴定出37个化合物，主要成分为萜烯化合物及其衍生物，柠檬烯为19．31％，里哪醇为15．26％，桧烯为13．60％。     

对位取代的四苯基卟啉衍生单酸的合成及有关的结构理论（英文）

报导了对位取代的四苯基卟啉衍生单酸的合成及表征,阐述了一些有关共轭叶琳平面环体系的结构理论。     

高效液相色谱法分析测定甘草、甘草酸制品及中成药中β－型甘草次酸的含量

 报道了应用高效液相色谱法，ＳＰＣ＿（１８）色谱柱，甲醇－水－冰醋酸（７９：２０：１，Ｖ／Ｖ）流动相，ＵＶ２５４ｎｍ，以标准甘草次酸为外标，测定了甘草、甘草酸制品及中成药中甘草次酸的含量。本法适用于测定不同中成药及甘草酸制品中的甘草次酸的含量，方法简便，快速准确。     

高效液相色谱法分析测定甘草、甘草酸制品及中成药中β－型甘草次酸的含量

报道了应用高效液相色谱法，ＳＰＣ＿（１８）色谱柱，甲醇－水－冰醋酸（７９：２０：１，Ｖ／Ｖ）流动相，ＵＶ２５４ｎｍ，以标准甘草次酸为外标，测定了甘草、甘草酸制品及中成药中甘草次酸的含量。本法适用于测定不同中成药及甘草酸制品中的甘草次酸的含量，方法简便，快速准确。     

11—脱氧甘草次酸衍生物的合成

用甘草次酸（Ａ）和甘草次酸甲酯（Ｂ）还原制得１１－脱氧甘草次酸（１）和１１－脱氧甘草次酸甲酯（２）。以此为原料进行酰化，合成了十种３－位酯化衍生物，再与碱金属氧化物反应合成了７种盐类衍生物。用ＩＲ，ＨＮＭＲ，ＭＳ和元素分析确证了它们的结构。     

11－脱氧甘草次酸衍生物的合成

用甘草次酸（Ａ）和甘草次酸甲酯（Ｂ）还原制得１１－脱氧甘草次酸（１）和１１－脱氧甘草次酸甲酯（２）。以此为原料进行酰化，合成了十种３－位酯化衍生物，再与碱金属氧化物反应合成了７种盐类衍生物。用ＩＲ、￣１ＨＮＭＲ、ＭＳ和元素分析确证了它们的结构。     

柱前衍生法在氨基酸分析测定中的应用

介绍了目前柱前衍生法分析氨基酸常用的几类衍生试剂及相应的衍生方法，并且比较了各类柱前衍生试剂的优缺点,对近期氨基酸分离分析中的色谱检测方法做了系统综述。     

新型荧光试剂柱前衍生化高效液相色谱荧光检测法测定醇类化合物

采用新型的紫外、荧光衍生试剂咔唑－9－乙基氯甲酸酯，对15种脂肪醇柱前衍生的反应条件，包括反应温度、催化剂的选择、衍生化时间等，进行了考察。结果表明：催化剂选用吡啶，反应温度80℃，时间15min，衍生化具有最大且恒定的检测响应。利用高效液相色谱对衍生产物进行分析，同时对衍生物的分离进行了优化选择，达到了较好的基线分离。检测限为13.3-93.5nmol/L。     

萘普生对映体的高效液相色谱分离

采用手性衍生化法，实验室合成了Ｌ－丝氨酸甲酯盐酸盐作为手性和衍生试剂，用于萘普生和－β－２－丙酸对映异构体的柱前衍生，以酰氯化间接衍生或缩水剂Ｎ，Ｎ‘－二环己基碳化二亚胺直接衍生形成酰胺非对映异构体对，然后用常规硅胶柱分离，同时利用色谱保留值规律和光谱特征吸收曲线综合进行定性分析。     

马钱子与甘草配伍前后生物碱成分的变化规律

采用电喷雾质谱技术和高效液相色谱法分别对马钱子配伍甘草前后主要生物碱的变化规律进行了系统研究。实验结果表明,马钱子配伍甘草后其主要生物碱士的宁和马钱子碱的含量均有不同程度的降低,其中士的宁的含量下降显著。电喷雾质谱的实验结果与高效液相色谱的结果相吻合,为进一步阐明甘草解马钱子类药物毒性和马钱子合理配伍用药提供了科学的实验依据。     

Field survey of Glycyrrhiza plants in central Asia (2). Characterization of phenolics and their variation in the leaves of Glycyrrhiza plants collected in Kazakhstan

A new prenylated flavanone, licoleafol, and a new prenylated dihydrostilbene, uralstilbene, together with four known compounds, 8-dimethylallyleriodictyol, sophoraflavanone B, gancaonin R, and 6-dimethylallyleriodictyol, were isolated from the leaves of Glycyrrhiza uralensis collected in Kazakhstan. HPLC analysis of the leaves of Glycyrrhiza plants collected in Kazakhstan showed that both G. uralensis-specific and Glycyrrhiza glabra-specific compounds were detected in the leaves of the morphologically intermediate-type plants, suggesting that the intermediate-type plant is a hybrid of G. glabra and G. uralensis. In addition, HPLC profiles of leaf extracts from offspring of intermediate-type plants were divided into the three types: the G. uralensis type, G. glabra type, and the intermediate type. From these results, it appears likely that the intermediate-type plant back-crosses with G. glabra and G. uralensis to generate a G. glabra-type plant and a G. uralensis-type plant, respectively.     

An automated method of on-line extraction coupled with flow injection and capillary electrophoresis for phytochemical analysis

In this study, an automated system for phytochemical analysis was successfully fabricated for the first time in our laboratory. The system included on-line decocting, filtering, cooling, sample introducing, separation, and detection, which greatly simplified the sample preparation and shortened the analysis time. Samples from the decoction extract were drawn every 5 min through an on-line filter and a condenser pipe to the sample loop from which 20-μL samples were injected into the running buffer and transported into a split-flow interface coupling the flow injection and capillary electrophoresis systems. The separation of glycyrrhetinic acid (GTA) and glycyrrhizic acid (GA) took less than 5 min by using a 10 mM borate buffer (adjusted pH to 8.8) and +10 kV voltage. Calibration curves showed good linearity with correlation coefficients (R) more than 0.9991. The intra-day repeatabilities (n = 5, expressed as relative standard deviation) of the proposed system, obtained using GTA and GA standards, were 1.1% and 0.8% for migration time and 0.7% and 0.9% for peak area, respectively. The mean recoveries of GTA and GA in the off-line extract of Glycyrrhiza uralensis Fisch root were better than 99.0%. The limits of detection (signal-to-noise ratio = 3) of the proposed method were 6.2 μg/mL and 6.9 μg/mL for GTA and GA, respectively. The dynamic changes of GTA and GA on the decoction time were obtained during the on-line decoction process of Glycyrrhiza uralensis Fisch root.     

Molecular Cloning and Expression Analysis of an Actin Gene from Chinese Licorice（Glycyrrhiza uralensis Fisch）

A PCR-based homologous cloning strategy was used to identify an actin gene from the roots of Chinese licorice(Glycyrrhiza uralensis Fisch). Results of sequence analysis indicate that a 1137 bp cDNA with an open reading frame encoding 377 amino acids,actin ortholog,GuActin,was successfully cloned and characterized(GenBank accession No. EU190972). Thus far,GuActin is the first actin of Chinese licorice that has been identified at a molecular level. Analysis by Northern blot shows that GuActin was expressed st...     

转换移动窗口因子分析法用于中药组合前后成分变化分析

以正十四烷为内标,采用气相色谱-质谱(GC/MS)联用技术对中药甘草(GUF)、甘遂(EKL)单味药材,以及其组成的药对(GUF-EKL)的挥发成分进行测定,基于一种新的化学计量学方法——转换移动窗口因子分析法(AMWFA)和直观推导式演进特征投影法(HELP)对产生的二维色谱/质谱数据同时进行分辨和解析,获取各个组分的纯色谱曲线和质谱,根据分辨得到的纯质谱在质谱库中进行相似检索以实现对组分的定性。利用AMWFA对组合前后的成分进行归属分析,然后采用面积归一法进行定量。分别在甘草、甘遂及其药对中鉴定出52、51和63个成分,占各自挥发油成分的84%、90%和75%。     

Studies on Triterpenoids and Flavones in Glycyrrhiza uralensis Fisch. By HPLC-ESI-MSn and FT-ICR-MSn

应用高效液相色谱质谱联用方法(HPLC-ESI-MSn)研究了甘草提取物中的七种化合物,四种三萜类化合物和三种黄酮类化合物。通过多极串联质谱(ESI-MSn)和多极串联傅里叶变换回旋共振质谱(FT-ICR-MSn)法研究了它们的碎裂规律。通过比较保留时间和质谱数据对上述七种化合物进行了归属,并阐述了其可能的质谱裂解途径。以上结果显示ESI-MSn和FT-ICR-MSn是非常有效的分析三萜类化合物和黄酮类化合物结构的工具。     

Preparative purification of glycyrrhizin extracted from the root of liquorice using high-speed counter-current chromatography

Glycyrrhizin is one of the main bioactive components in liquorice (Glycyrrhiza uralensis Fisch) which has recently been found to be highly active in inhibiting replication of the severe acute respiratory syndrome (SARS)-associated virus. The separation and purification of glycyrrhizin from a methanol-water (70:30 (v/v)) extract of liquorice roots was achieved using high-speed counter-current chromatography. The separation was performed at a preparative scale in a one-step separation with a two-phase solvent system composed of ethyl acetate-methanol-water (5:2:5 (v/v)). The lower phase was used as the mobile phase in the head-to-tail elution mode. The present method yielded 42.2 mg glycyrrhizin at 96.8% purity from 130 mg of the crude exact with 95.2% recovery as determined by HPLC analysis.     

甘草苷在玻碳电极上的电化学行为及其测定

在pH 3.00的B-R缓冲溶液中,采用差分脉冲伏安法(DPV)、线性扫描伏安法(LSV)和循环伏安法(CV)研究了甘草苷在玻碳电极上的电化学行为, 建立了测定甘草苷的DPV法。实验结果表明,甘草苷于1.16 V (vs.Ag/AgCl)处产生一个氧化峰,峰电流和甘草苷的浓度在2.00×10-6~3.50×10-5 mol/L范围内呈良好的线性关系,检出限为8.25×10-7 mol/L。该法用于实际样品甘草、胃康灵和逍遥丸中黄酮含量的测定(以甘草苷为对照品),平均回收率分别为97.1%、98.9%和102.0%。此外对电极反应机理作了初步探讨。     

Tracking antiangiogenic components from Glycyrrhiza uralensis Fisch. based on zebrafish assays using high-speed countercurrent chromatography

Natural products are some of the most important sources of lead compounds for drug discovery. The advanced isolation technique of lead compounds of natural origin using therapeutically relevant bioassays is capable of enhancing work efficiency from complex multiconstituent extracts. In the present study, a bioassay-guided isolation strategy combined with bioactivity screening was used to identify novel angiogenesis inhibitors from licorice (Glycyrrhiza uralensis Fisch.) based on the zebrafish model and rapid preparative separation by high-speed countercurrent chromatography. Zebrafish embryos at 24 h postfertilization were chosen as the angiogenesis inhibition model for bioactivity screening. A solvent system (n-hexane-ethyl acetate-methanol-water) with different ratios was optimized and applied in the high-speed countercurrent chromatography separation of two fractions, Fr5 and Fr6, from the ethyl acetate extract of licorice. Blood circulation and vascular outgrowth in intersegmental vessels were found to be simultaneously inhibited by isoliquiritigenin and isolicoflavonol in a dose-dependent manner. Thus, these two compounds were identified and considered as active inhibitors against angiogenesis. These experimental results indicate that zebrafish bioassays combined with high-speed countercurrent chromatography may provide an alternative pathway for the rapid isolation of bioactive natural products.     

A novel biflavonoid from roots of Glycyrrhiza uralensis cultivated in China

A novel biflavonoid named licobichalcone was isolated from the roots of Glycyrrhiza uralensis cultivated in China, along with twelve known compounds, including five chalcones, two isoflavones, two flavanones, two flavones and one pterocarpan. Their structures were respectively elucidated on the basis of chemical and spectroscopic evidence.