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1.
银杏叶黄酮类化合物的提取分离Ⅰ.银杏黄酮化合物的提取   总被引:16,自引:1,他引:15  
银杏叶为银杏科银杏属植物银杏(Ginkgo biloba L.)的叶子,银杏在植物学和化学上占有重要地位。据《本草纲目》记载,银杏果具有敛肺平喘,止遗尿,白带作用,近年来,国内外学者对银杏提取物(GBE)进行了大量的研究,发现其主要药用成分之一为黄酮类化合物,以银杏 叶为原料提取制成的药物,用于对心血管,脑血管,动脉硬化,高血压等疾病的治疗,有其他药物不能达到的特殊疗效^[1-4]。另外,银杏制剂长期服用几乎没有毒副作用,银杏叶制品还可用于生物农药,保健食品,化妆品等方面,如何从银杏叶中提取有效成分有研究的关键。银杏叶黄酮化合物的提取包括银杏叶黄酮化合物的浸取和浸出液的富集分离两大部分。本文主要讨论银杏叶黄酮类化合物的浸取。  相似文献   

2.
近红外光谱法同时测定银杏提取液中总黄酮和总内酯含量   总被引:12,自引:0,他引:12  
胡钢亮  吕秀阳  罗玲  徐铸德 《分析化学》2004,32(8):1061-1063
采用傅里叶变换近红外透射光谱和偏最小二乘法,对银杏提取液中总黄酮和总内酯的含量进行了定量测定。所建立的数学模型对校正集样本的银杏总黄酮和总内酯复相关系数(MR)分别为O.998和o.986;对预测集样本的银杏总黄酮和总内酯复相关系数分别为0.983和0.971,标准回收率分别为95.71%~103.3%和95.29%~104.6%,相对标准偏差(RSD)分别为2.44%和3.19%。结果表明,近红外光谱测定银杏提取液中总黄酮和总内酯含量具有快速、准确的优点,有望应用于银杏提取过程的中间控制和大批量产品的检测。  相似文献   

3.
油菜蜂花粉黄酮含量的HPLC测定   总被引:8,自引:1,他引:7  
以95%乙醇为溶剂,采用索氏提取器提取青海产油菜蜂花粉中的黄酮类化合物,将黄酮提取物中的黄酮甙水解为黄酮甙元后,利用HPLC法测定其中槲皮素、山萘酚、异鼠李素含量。结果表明,青海油菜蜂花粉中槲皮素、山萘酚、异鼠李素的平均含量分别为0.928%、0.295%、0.0834%,换算成总黄酮含量为3.28%。  相似文献   

4.
基于在碱性条件下,银杏黄酮对CIO^--鲁米诺体系有显著的抑制作用,结合反相流动注射技术,建立了流动注射.抑制化学发光测定银杏提取物中的银杏黄酮。银杏黄酮质量浓度在0.4~14.0μg/ML范围与相对发光强度呈线性关系,检出限为0.06μg/ML,采样频率为120次/h,对10.0μg/ML的银杏黄酮平行测定11次,其RSD为1.2%,回收率为98、0%~104%。该方法可用于银杏黄酮制剂的测定。  相似文献   

5.
生物技术培养银杏发根中的黄酮分析研究   总被引:2,自引:0,他引:2  
本文研究了银杏发根中黄酮含量的高效液相色谱(HPLC)分析方法,改进了样品预处理过程,实行提取、水解同步进行,并与天然银杏树叶中的黄酮进行了对照,分析结果表明,采用生物技术培养的银杏发根中确实含有银杏黄酮。  相似文献   

6.
银杏根中黄酮类化合物的分离分析   总被引:5,自引:1,他引:4  
采用丙酮浸泡、回流从银杏根中提取得到黄酮,以HPLC法分离测定其中的槲皮素含量。实验结果表明:银杏根黄酮存在槲皮素甙,不含山奈酚、异鼠李素等物质。  相似文献   

7.
采用正交试验法,优选大孔树脂提纯罗布麻中总黄酮的最佳工艺。以芦丁为对照品,采用分光光度法进行测定,以罗布麻中总黄酮回收率为考察指标,对影响总黄酮纯化工艺的因素进行研究;在单因素实验基础上,选择树脂种类、p H值、料液浓度、解吸液乙醇浓度等4个因素进行正交试验,研究不同因素交互作用及其对黄酮回收率的影响,结合吸附和解吸流速,确定罗布麻总黄酮提纯的最佳工艺;用高效液相色谱法对提纯前后芦丁含量进行比较,验证纯化效果。经正交试验,确定最佳工艺参数如下:AB-8树脂,料液浓度为0.125mg/mL,p H=5,吸附流速为3mL/min,解吸液乙醇浓度为80%,解吸流速为5mL/min。在此工艺条件下,总黄酮产率为2.64%,总黄酮含量由10.1mg/g提高到378.6mg/g;经高效液相色谱法计算,芦丁含量由6.3mg/g提高到185.6mg/g。  相似文献   

8.
银杏叶SF-CO_2萃取物与残叶银杏黄酮的HPLC分析   总被引:3,自引:0,他引:3  
银杏叶用SF -CO2 -CH3 CH2 OH体系萃取后 ,用HPLC法分析萃取物与残叶中银杏黄酮苷与黄酮苷元的含量。结果表明 ,有夹带剂时可萃取黄酮苷元 ;无论有无夹带剂银杏黄酮苷都残留在萃取残叶中。  相似文献   

9.
刺五加味中黄酮类化合物的分析   总被引:9,自引:0,他引:9  
陈貌连  宋凤瑞等 《分析化学》2002,30(6):《分析化学》-2002年30卷6期-690-694-页-《分析化学》-2002年30卷6期-690-694-页
利用电喷雾多级串联质谱(ESI-MS^n)技术,分析了刺五加叶中黄酮类化合物,并根据黄酮类化合物的特征显色反应,采用紫外-可见分光光度法,对刺五加叶中总黄酮的含量进行了测定。分析结果表明:刺五加叶含有槲皮素及其相关的黄酮甙类化合物,其含量达37.25%。  相似文献   

10.
研究鸡足山耳蕨中总黄酮的提取及其抗氧化性.采用70%乙醇提取鸡足山耳蕨中总黄酮,用NaNO2Al(NO3)3-NaOH分光光度法测定黄酮含量,将提取液采用Fenton体系、普鲁士蓝法进行体外抗氧化活性研究,用硫代巴比妥酸(TBA)分光光度法研究其对羟自由基·OH引发DNA氧化损伤的抑制作用.结果表明样品中总黄酮含量为4.98%,回收率99.78%( RSD=1.06%,n=5).总黄酮浓度为90μg/mL时,对·OH的清除率可达36.2%;浓度为87.5μg/mL时,对羟自由基引发DNA损伤的抑制率可达93.0%.说明鸡足山蕨中总黄酮对羟自由基有较好的清除能力,对DNA氧化损伤有显著抑制作用.  相似文献   

11.
A novel chromatographic process for purification of α1 proteinase inhibitor (α1-PI) from Cohn fraction IV-1 paste is described. This process has been successfully scaled up to 50-l columns. It involves DEAE chromatography, sulfopropyl (S) cation chromatography, tri-n-butyl phosphate (TNBP)–cholate treatment, a second S cation chromatography, freeze–drying and dry-heat. The process has been optimized for purity, yield, lipid removal, chemical usage and water consumption. Filtration after TNBP–cholate treatment plays a key role in ensuring a low lipid content in the final product. Pre-equilibration with high salt buffer is necessary to reduce the water consumption significantly during the ion-exchange chromatography equilibration step. The final product is approximately 95% pure by sodium dodecyl sulfate–polyacrylamide gel electrophoresis, with a 64% to 70% yield from IV-1 paste.  相似文献   

12.
促卵泡激素的径向色谱纯化工艺   总被引:1,自引:0,他引:1  
郭立安  阎哲  杨晓东  褚西秦  徐海峰 《色谱》2000,18(6):577-579
 比较了径向离子交换色谱与经典离子交换色谱在纯化工艺放大过程中的分离效果 ,证实了径向色谱比经典色谱更适合于促卵泡激素 (FSH)的纯化 ,并建立了适合于大规模生产FSH的径向色谱纯化新工艺。纯化后FSH的比活性为 180IU/mg ,活性回收率为 5 6 % ,产品质量符合国家药典规定。  相似文献   

13.
In the large-scale manufacturing and purification of protein therapeutics, multiple chromatography adsorbent lots are often required due to limited absorbent batch sizes or during replacement at the end of the useful column lifetime. Variability in the adsorbent performance from lot to lot should be minimal in order to ensure that consistent product purity and product quality attributes are achieved when a different lot or lot mixture is implemented in the process. Vendors of chromatographic adsorbents will often provide release specifications, which may possess a narrow range of acceptable values. Despite relatively narrow release specifications, the performance of the adsorbent in a given purification process could still vary from lot to lot. In this case, an alternative use test (one that properly captures the lot to lot variability) may be required to determine an acceptable range of variability for a specific process. In this work, we describe the separation of therapeutic protein monomer and aggregate species using hydrophobic interaction chromatography, which is potentially sensitive to adsorbent lot variability. An alternative use test is formulated, which can be used to rapidly screen different adsorbent lots prior to implementation in a large-scale manufacturing process. In addition, the underlying mechanism responsible for the adsorbent lot variability, which was based upon differences in protein adsorption characteristics, was also investigated using both experimental and modeling approaches.  相似文献   

14.
Pharmaceutical development currently relies on quality separation methods from early discovery through to line-of-site manufacturing. There have been significant advancements made regarding the column particle packing, internal diameter, length connectivity, the understanding of the impact key parameters like void volume, flow rate, and temperature all that affects the resultant separation quality, that is, resolution, peak shape, peak width, run time, and signal-to-noise ratio. There is however a strong need to establish better alternatives to large bulky high-performance liquid chromatography racks either for process analytical reaction monitoring or mass spectrometry analysis in establishing product quality. Compact, portable high-pressure liquid chromatography can be a more efficient alternative to traditional ultra-high pressure liquid chromatography and traditional liquid chromatography. The compact versatile instrument evaluated here allows good separation control with either the on-board column with fixed ultra-violet wavelength cartridge or for use with a high-resolution mass spectrometry. Significant space reduction results in greener lab spaces with improved energy efficiency for smaller labs with lower energy demands. In addition, this compact liquid chromatography was used as a portable reaction monitoring solution to compare forced degradation kinetics and assess portable liquid chromatography-mass spectrometry capability for the analyses required for pharmaceutical drug product testing.  相似文献   

15.
Monoclonal antibodies are tetrameric complex proteins, primarily produced using mammalian cell culture. Attributes such as titer, aggregates, and intact mass analysis are monitored during process development/optimization. In the present study, a novel workflow such that the Protein-A affinity chromatography is performed in the first dimension for purification and titer estimation, whereas size exclusion chromatography is employed in the second dimension to characterize size variants using native mass spectrometry. The present workflow offers a significant advantage over the traditionally used standalone Protein-A affinity chromatography followed by size exclusion chromatography analysis in that it can monitor these four attributes in 8 min while requiring a minimal sample size (10–15 μg) and not requiring any manual peak collection. In contrast, the traditional standalone approach requires manual collection of eluted peaks in Protein-A affinity chromatography followed by buffer exchange to a mass-compatible buffer, which can take up to 2–3 h with considerable risk of sample loss, degradation, and induced modifications. As the biopharma industry moves to make analytical testing efficient, we believe that the approach proposed here would be of significant interest due to its ability to monitor multiple process and product quality attributes in a single workflow and via rapid analysis.  相似文献   

16.
This work describes the analysis of a pyrolysis product of a lignite sample obtained from the Turkish Goynuk reserve. The aliphatic, aromatic and polar compounds present in the tar are separated and identified by various chromatographic techniques: Capillary gas chromatography/mass spectrometry (GC/MS), on-line high performance microbore liquid chromatography/capillary gas chromatography (LC/GC) and capillary supercritical fluid chromatography (SFC). The suitability of each technique for this particular application is discussed, and semi-quantitative results are presented for the major components detected.  相似文献   

17.
不用化学试剂只用水的离子色谱(Reagent Free Ion Chromatography,RFIC)是2003年才问世的新一代色谱技术,荣获2003年Pitteon会议金奖。本文将详细讨论这一技术的基本原理和应用。  相似文献   

18.
亲和色谱纯化蛋白质新进展   总被引:6,自引:2,他引:4  
韩金玉  那平  元英进 《色谱》1996,14(6):447-450
 通过对35篇文献的综述,介绍了亲和色谱技术的新进展  相似文献   

19.
Important objectives of a high‐performance liquid chromatography preparative process are: purity of products isolated, yield, and throughput. The multidimensional preparative liquid chromatography method used in this work was developed mainly to increase the throughput; moreover purity and yield are increased thanks to the automated collection of the molecules based on the intensity of a signal generated from the mass spectrometer detector, in this way only a specific product can be targeted. This preparative system allowed, in few analyses both in the first and second dimensions, the isolation of eight pure compounds present at very different concentration in the original sample with high purity (>95%) and yield, which showed how the system is efficient and versatile. Pure molecules were used to validate the analytical method and to test the anti‐inflammatory and antiproliferative potential of flavonoids. The contemporary presence, in bergamot juice, of all the flavonoids together increases the anti‐inflammatory effect with respect to the single compound alone.  相似文献   

20.
Protein A resins are often reused for multiple cycles to improve process economy during mAb purification. Significant reduction in binding capacity and product recovery are typically observed due to the presence of unwanted materials (foulants) deposited on the resin upon reuse. In this paper, we have used a wide spectrum of qualitative and quantitative analytical tools (particle size analysis, HPLC, fluorescence, SEM, MS, and FTIR) to compare the strengths and shortcomings of different analytical tools in terms of their capability to detect the fouling of the resin and relate it to chromatographic cycle performance. While each tool offers an insight into this complex phenomena, fluorescence is the only one that can be used for real‐time monitoring of resin fouling. A correlation could be established between fluorescence intensity and the process performance attributes (like yield or binding capacity) impacted upon resin reuse. This demonstration of the application of fluorescence for real‐time monitoring correlated empirically with process performance attributes and the results support its use as a PAT tool as part of a process control strategy. While the focus of this paper is on fouling of protein A chromatography resin, the approach and strategy are pertinent to other modes of chromatography as well.  相似文献   

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