枫蓼肠胃康口服液HPLC指纹图谱研究

建立了一种整体定性鉴别和指标成分定量的HPLC指纹图谱方法,对由牛耳枫和辣蓼两味药材组成的枫蓼肠胃康口服液原料及成品进行了指纹图谱研究,并测定了指标成分芦丁、金丝桃苷和异鼠李素的含量。采用Waters ODS C18色谱柱(250 mm×4.6 mm I.D.5μm),用含甲醇和甲酸溶液作为流动相,进行梯度洗脱,并对原料和成品的相应色谱峰进行归属鉴别。结果显示芦丁、金丝桃苷和异鼠李素得到了满意的线性范围,相关系数均大于0.999。按照SFDA的要求,对原料和成品的色谱指纹图谱采用相关系数法和夹角余弦法两种数学方法计算它们的相似度,两种计算方法相似度均不小于0.852。表明建立的枫蓼肠胃康口服液的定性定量方法显著优于传统的质量控制方法。     

HPLC法测定18种菊科植物中总黄酮醇苷含量研究

目的:建立测定青海产18种菊科植物中总黄酮醇苷含量的方法。方法:Reprosil C18-AQ色谱柱(4.6 mm×250 mm,5μm),流动相甲醇-0.2%甲酸溶液(48∶52),检测波长360 nm,流速1.0 mL/min,柱温40℃,进样量10μL。结果:槲皮素、山柰素和异鼠李素3种黄酮类化合物在1.06～212、1.06～212、0.93～186μg/mL浓度范围内均线性关系良好。本方法精密度、稳定性和重复性良好。结论:该方法准确稳定,重复性好,可用于菊科植物的质量控制。     

一测多评法测定番石榴叶中6种黄酮类成分的含量

为建立同时测定番石榴叶中6种黄酮类成分(金丝桃苷、异槲皮苷、瑞诺苷、番石榴苷、萹蓄苷、槲皮素)的一测多评法。本研究以金丝桃苷为内参物,采用HPLC法,确定金丝桃苷与另外5种成分的相对校正因子,并通过获得的校正因子计算后5种成分的量;同时采用外标法测定11批番石榴叶的含量。结果表明11批番石榴叶的QAMS法与外标法测定结果间无显著性差异,证明该法可用于番石榴叶6种黄酮类成分的定量分析。     

绿肉山楂叶中五种黄酮类成分含量动态变化

为充分利用山楂叶用资源,采用反相高效液相色谱法,以ZORBAX Extend-C18色谱柱（250×4.6 mm,5 μm）,乙腈-0.5%磷酸水溶液梯度洗脱,流速1.0 mL·min^-1,检测波长345 nm,柱温25℃,对不同生长时期的绿肉山楂叶中牡荆苷、牡荆素2″-O-鼠李糖苷、金丝桃苷、芦丁和槲皮素含量进行测定。结果表明,在此分析检测条件下牡荆苷、牡荆素 2″-O-鼠李糖苷、金丝桃苷、芦丁和槲皮素的精密度、重复性、稳定性及平均加样回收率试验的RSD值均小于3%,方法准确可靠。绿肉山楂叶中含有的黄酮类成分主要以牡荆苷和金丝桃苷为主,且二者含量变化规律与其总黄酮含量变化相似,均在10月初含量达到最高;此时采摘,其质量完全符合《中国药典》的有关规定,故绿肉山楂可作为一种新的药用资源来进一步开发利用。     

不同采收期罗布麻和白麻药材化学成分的差异分析

建立高效液相色谱法,分别测定不同采收期的新疆产罗布麻和白麻药材中绿原酸、金丝桃苷、异槲皮苷、三叶豆苷、紫云英苷、芦丁和白麻苷的含量,进而分析2种药材的最佳采收期。发现不同采收期的新疆产罗布麻和白麻药材中绿原酸、金丝桃苷、异槲皮苷、三叶豆苷、紫云英苷、芦丁和白麻苷的含量存在一定差异,并且罗布麻和白麻呈现出不同特点。以《中国药典》中罗布麻含量测定项下的金丝桃苷为指标,罗布麻和白麻的最佳采收期都是6、7月;但是,以7个成分的总含量和6个黄酮的总含量为指标,罗布麻的最佳采收期是8、9月,白麻的最佳采收期仍是6、7月。该结果可为确定罗布麻和白麻药材的采收时间提供一定参考。     

水烛香蒲不同部位黄酮类化合物的动态分析

为了分析水烛香蒲花粉和茎叶中黄酮类成分,以及不同生长期、不同部位中香蒲新苷、异鼠李素-3-O-新橙皮苷和异鼠李素含量。该文采用UPLC-Q-TOF-MS进行定性分析,结合HPLC法对水烛香蒲不同部位中黄酮类化合物含量进行分析评价,色谱条件为PRAZIS C_(18)柱(250 mm×4.6 mm,5μm),以乙腈-0.05%磷酸为流动相,梯度洗脱,体积流量1.0 mL·min~(-1),检测波长254 nm,柱温30℃。结果表明:(1)花粉及茎叶中共解析出42个化合物,其中8个化合物在不同部位中有差异。(2)同一生长环境的水烛香蒲不同生长时期、不同部位中3种黄酮类化合物的含量差异较大。(3)异鼠李素-3-O-新橙皮苷及异鼠李素在香蒲的发育生长过程中含量呈先增加后下降的趋势,茎叶内的这两种成分含量下降明显;在花粉中,香蒲新苷和异鼠李素-3-O-新橙皮苷含量急剧上升,一周内达到峰值;茎叶中香蒲新苷含量较低,在大多数样品中未检出。该研究所建立的测定方法简便、重现性好,并对水烛香蒲中黄酮类成分的含量变化规律进行了研究,对花粉及茎叶中化合物差异进行了分析,为蒲黄的合理采收及香蒲植物的资源化利用提供了科学依据。     

毛细管区带电泳法测定油菜蜂花粉中黄酮苷元含量

本文研究了芦丁、槲皮素、山萘酚、异鼠李素四种黄酮类化合物在毛细管区带电泳中的迁移行为,考察了缓冲溶液pH值、其离子浓度、有机添加剂、电压、温度等对分离的影响。结果发现在35mmol／L硼砂缓冲溶液,pH8．4,10％乙腈作为添加剂,20℃,25kV条件下,四种黄酮在14min内实现了基线分离。利用该方法测定青海产油菜蜂花粉中黄酮苷元含量,结果令人满意。     

山豆根化学成分研究

利用多种柱层析方法,从山豆根中分得5个化合物。经过理化及波谱分析,分别鉴定为L-广高丽槐素(1)、红车轴草苷(2)、槲皮素(3)、芦丁(4)和异鼠李素-3-芸香糖甙(5)。其中化合物3,5为首次从该植物中分离得到。关键词：山豆根;L-高丽槐素;红车轴草苷;槲皮素;芦丁;异鼠李素-3-芸香糖甙     

UPLC-MRM-MS法测定头花蓼药材中7个指标成分

建立头花蓼药材中没食子酸、原儿茶酸、陆地棉苷、槲皮苷、儿茶素、槲皮素-3-O-(2″-没食子酰基)-鼠李糖苷及槲皮素的UPLC-MRM-MS检测方法。色谱采用Waters BEH C18(2.1 mm×50 mm,1.7μm)色谱柱,以0.1%甲酸乙腈-0.1%甲酸水溶液为流动相,梯度洗脱,质谱采用多反应离子监测(MRM)检测。没食子酸、原儿茶酸、陆地棉苷、槲皮苷、儿茶素、槲皮素-3-O-(2″-没食子酰基)-鼠李糖苷及槲皮素分别在0.136~32.965、0.031~7.481、0.022~5.300、0.076~18.433、0.085~20.737、0.017~4.147、0.128~31.029μg/m L浓度范围线性关系良好,平均回收率为91.23%~105.33%,RSD3%,精密度、重复性和稳定性良好。此方法操作简便,快速,灵敏度高,可用于头花蓼药材中主要活性成分的含量测定,并为头花蓼药材质量控制提供了新方法。     

毛绞股蓝化学成分研究——Ⅰ.黄酮类化合物

本文首次从毛绞股蓝 Gynostemma pubescens(Gagnep.)C.Y,Wu 的茎叶中分得四种黄酮类成分,经理化方法和光谱数据鉴定为:异鼠李素(isorhamnetin),檞皮素(quercetin),异鼠李素-3-0-芸香糖甙(isorhamnetin-3-0-rutinoside)和芦丁(rutin)。     

红凤菜新鲜茎叶中总黄酮提取物的LC-MS分析

红凤菜（Gynura bicolor DC.）为菊科（Compositae）菊三七属（Gynura Cass.）植物,别名血皮菜、观音菜、观音苋、紫背天葵等,主要分布于中国南方各地,全草均可入药[1];也可作为蔬菜食用,在国内多个地区均有栽培和销售。目前已知红凤菜含有黄酮类、酚性酸类、萜类、甾醇类、脂肪酸类、生物碱类及花青素类等[2-7]成分。由于黄酮类成分多具有保护心血管、抗肿瘤、抗糖尿病、抗氧化、抗炎和抗病毒等作用[8],因此对红凤菜中黄酮类成分的研究具有深度开发价值。     

The analgesic action of some flavonoids in the hot plate test.

Albino-Swiss male mice were tested in the hot plate test. Oligomeric procyjanidin (OL-1), rutin, quercetin, hyperoside and vitexin rhamnoside were administered intraperitoneally in doses 3.5 and 10 mg/kg. It was found that OL-1, rutin and hyperoside but not vitexin rhamnoside exert analgesic action, whereas quercetin even decreases the pain threshold level. The mechanism of the analgesic action of flavonoids remains to be explained.     

Variation of Bioactive Compounds in Hypericum perforatum Growing in Turkey During Its Phenological Cycle

The present study was conducted to determine phenologic and morphogeneUc variation of hyperlcln, chlorogenlc acid and flavonoids, as rutin, hyperoside, apigenin-7-O-glucoside, quercitrin, quercetin content of Hypericum perforatum L. growing in Turkey. Wild growing plants were harvested at vegetative, floral budding, full flowering, fresh frulUng and mature fruiting stages and dissected into stem, leaf and reproductive tissues and assayed for bioacUve compounds by the High performance liquid chromatography （HPLC） method. Hypericin concentration ranged between 0 and 2.73 mg/g DW, chlorogenic acid 0.00-3.64 mg/g DW, rutin 0.00-3.36 mg/g DW, hyperoside 0.04- 22.42 mg/g DW, quercitrin 0.03-3.46 mg/g DW and quercetin 0.04-1.02 mg/g DW depending on ontogenetic and morphogenetic sampling. Leaves were found to be superior to stems and reproductive parts with regard to phenolic accumulation for all compounds tested while flowers accumulated the highest levels of hypericln. Quercltrln, quercetln and hypericin content in all tissues increased with advancing of developmental stages and reached their highest level during flower ontogenesis. Similarly, chlorogenic acid, hyperoside and apigenin-7-O-glucoside content in different plant parts increased during plant development, however, the highest level was observed at different stages of plant phenology for each tissue. Chlorogenic acid was not detected in stems, leaves and reproductive parts in several stages of plant phenology and its variation during plant growth showed inconsistent manner. In contrast to the other compounds examined, rutin content of stems and leaves decreased with advanc- ing of plant development and the highest level for both tissues was observed at the vegetative stage. However, content of the same compound in reproductive parts was the highest at mature fruiting. The present findings might be useful to obtain increased concentration of these natural compounds.     

Flavonoid glycosides and phenolic acids from Ehretia thyrsiflora

Chemical constituents of the leaves of Ehretia thyrsiflora were continuously investigated. Twelve compounds including six flavonoids and six phenolic acids, isoquercetrin, hyperoside, trifolin, astragalin, kaempferol 3-O-arabinosylgalactoside, quercetin 3-O-arabinosylgalactoside, rosmarinic acid, cinnamic acid, icariside E5, ferulic acid, α-hydroxydihydrocaffeic acid, lithospermic acid B were first isolated from this species. The considerable phenolic compounds existed in this species have important systematic significance in the argument of the family the Boraginaceae.     

Variation of bioactive substances and morphological traits in Hypericum perforatum populations from Northern Turkey

Hypericum perforatum L. has become one of the leading plant-based dietary supplements worldwide and its biological activities have been mainly attributed to hypericin and phenolic contents. The present study was conducted to determine chemical and morphological variability of H. perforatum sampled from different locations of Northern Turkey. The populations were investigated according to the hypericin, chlorogenic acid and the flavonoids, namely rutin, hyperoside, apigenin-7-O-glucoside, quercitrin and quercetin contents and morphological characters including leaf dark gland density, leaf area, leaf length/width ratio and plant height. Significant chemical and morphological variations were detected among the populations. Hypericin content among populations ranged between 0.44 and 2.82 mg/g dry weight, chlorogenic acid between 0.0 and 1.86 mg/g dry weight, rutin between 0.0 and 8.77 mg/g dry weight, hyperoside between 5.41 and 22.28 mg/g dry weight, quercitrin between 1.64 and 3.98 mg/g dry weight and quercetin between 1.01 and 1.76 mg/g dry weight. Hypericin content was found to be correlated positively with leaf dark gland density, however, negatively with leaf area and no correlation was detected between the other morphological traits and bioactive substances examined.     

青海油菜蜂花粉黄酮类化合物含量的研究

采用正交试验设计,研究了青海油菜蜂花粉中黄酮类化合物的最佳提取条件,分别采用HPLC法和比色法测定了黄酮类化合物的含量。最佳提取条件是选用95％的乙醇作为溶剂,以10倍总量的乙醇用量,水浴热回流提取。以槲皮素、山奈酚、异鼠李素为对照品,采用HPLC法,测定出黄酮类化合物平均含量为3．194％;以芦丁为对照物,采用比色法,测定出总黄酮平均含量为3．70％。     

荷花花粉的类黄酮组成

利用超高效液相色谱质谱联用(I-Class UPLC/Xevo TQ MS)技术, 对50个品种荷花干燥花粉中的类黄酮代谢产物进行了分离及结构鉴定。结果表明, 在荷花(Nelumbo nucifera)花粉中检测到了13种黄酮醇和2种黄酮, 这15种类黄酮化合物均为首次从荷花花粉中检出, 其中槲皮素3-O-葡萄糖醛酸苷(quercetin 3-O-glucuronide)、槲皮素3-O-新橙皮糖苷(quercetin 3-O-rhamnopyranosyl-(1→2)-glucopyranoside)以及槲皮素3-O-阿拉伯糖-(1→2)-半乳糖苷(quercetin 3-O-arabinopy- ranosyl-(1→2)- galactopyranoside)含量较高, 且在所有品种中均有检出。不同品种花粉中检测到的类黄酮总含量(TF)差异较大, 绯云千叶类黄酮总含量最高, 为281.08 mg∙100 g^-1; 仙女散花最低, 仅为82.64 mg∙100 g^-1。通过聚类分析, 将50个品种聚为4组, B组类黄酮化合物种类最多, 而且该组总类黄酮含量最高, 其中绯云千叶、伯里小姐和蜀红莲的干燥花粉中总类黄酮含量均超过200 mg∙100 g^-1, 可推荐为采集荷花花粉用的优良品种。     

迎春花中黄酮类化合物含量的研究

以75％乙醇为溶剂,索氏提取器提取,采用比色法和HPLC法研究了迎春花中黄酮类化合物的含量。以芦丁为对照物,比色法测定出其花、叶、茎中总黄酮的含量分别为13．7％、16．2％、6．77％．RSD分别为2．63％、2．57％、2．96％;以槲皮素、山奈素、异鼠李素为对照物,HPLC法测定出其花、叶、茎中的黄酮总量,以甙元计分别为4．205％、3．371％、1．703％,RSD分别为1．76％、1．58％、1．98％。     

Biologically active substances isolated from Hypericum attenuatum Choisy

Four dianthrones, two oxymethylanthraquinones, two reductive forms of anthraquinones and five flavonoids have been isolated from the plant source Hypericum attenuatum Choisy (Guttiferae) firstly investigated for these substances contents. Dianthrones pseudohypericin, protohypericin, protopseudohypericin, oxymethylanthraquinones frangulaemodin, frangulin, reductive anthraquinones emodin anthrone, emodin anthranol, and flavonoids quercetin, quercitrin, isoquercitrin, rutin have been identified for the first time. High hyperoside contents in herb of Hypericum attenuatum is established.     

Variation of bioactive secondary metabolites in <Emphasis Type="Italic">Hypericum origanifolium</Emphasis> during its phenological cycle

The genus Hypericum has received considerable interest from scientists, as it contains the variety of structurally diverse natural products which possess a wide array of biological properties. The present study was conducted to determine ontogenetic and morphogenetic variation of hypericin, chlorogenic acid and flavonoids, as rutin, hyperoside, apigenin-7-O-glucoside, quercitrin and quercetin content in Hypericum origanifolium growing in Turkey. Wild growing plants were harvested at vegetative, floral budding, full flowering, fresh fruiting and mature fruiting stages and dissected into stem, leaf and reproductive tissues and assayed for bioactive compounds by HPLC method. Hypericin, quercetin and quercitrin content in whole plant increased during course of ontogenesis and the highest level was reached in blooming stage. On the contrary, hyperoside content of whole plant decreased linearly with advancing of development stages and the highest level was observed at vegetative stage. Plants produced similar amount of chlorogenic acid at all stages of plant phenology except for mature fruiting at which the amount of this compound was decreased sharply. Among different tissues, reproductive parts accumulated the highest level of hypericin, quercetin and quercitrin, however, leaves produced substantially higher amount of chlorogenic acid and hyperoside. Rutin and apigenin-7-O-glucoside were detectable in all tissues only during fruit maturation. The presence and variation of these bioactive substances in H. origanifolium were reported for the first time.