首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 169 毫秒
1.
从银杏叶中分离制备高纯度双黄酮对照品,探讨其抗氧化活性强弱。以60%乙醇-水提取的银杏叶浸膏为原料,反溶剂沉淀得到含量80.40%的双黄酮粗品,再以甲醇-水为流动相,半制备色谱梯度洗脱。结果得到了4种符合中药化学对照品要求的高纯度双黄酮,在最佳制备条件下,4种双黄酮纯度:阿曼托黄素(98.45%)、白果素(98.66%)、银杏黄素异构体(98.87%)、金松双黄酮(99.29%),其产率(mg/kg)分别为:22.5、23.8、192.5、71.8,考察了它们的抗氧化活性,并采用60%乙腈和有机酸水溶液对银杏黄素异构体进行了完全分离。建立的制备方法快速简便,所得单组分双黄酮纯度、产量高。本工作为单组分银杏双黄酮新药的研究与开发提供重要的技术支持。  相似文献   

2.
建立丹参提取物中酚酸类含量的快速检测方法。以丹酚酸B为对照,采用分光光度法于482 nm处测定丹参提取物中酚酸类的含量。结果表明丹酚酸B在0.0782~1.0166 mg(r=0.9977)范围内线性关系良好,回收率为101.652%,RSD值为0.81%(n=9)。该提取物中酚酸类含量测定结果为19.636%。该方法快速简便、准确、重现性好,可作为快速检测丹参中总酚酸含量的方法。  相似文献   

3.
采用快速制备液相色谱从库拉索芦荟中高效分离制备10-羟基芦荟大黄素苷A和B。以库拉索芦荟药材粉甲醇提取物为原料,采用快速制备液相色谱,EYELA柱(300 mm×20 mm i.d.,20~45μm),甲醇-水为流动相(35∶65,v/v)等度洗脱,流速10 mL/min,检测波长356 nm,对芦荟样品进行分离制备,得到2种化合物单体,经UV、旋光度、HRMS和NMR鉴定,HPLC测定纯度,2个化合物分别为10-羟基芦荟大黄素苷B(98.9%)和10-羟基芦荟大黄素苷A(98.2%)。该方法简便、快速,所得产物纯度较高,可用于对照品的制备和药理毒理活性研究。  相似文献   

4.
采用高速逆流色谱(HSCCC)技术从蛹虫草子实体粗提物中分离制备高纯度虫草素和N6-(2-羟乙基)-腺苷。利用高效液相色谱(HPLC)测定目标产物在溶剂体系中的分配系数,优化HSCCC分离虫草素和N6-(2-羟乙基)-腺苷的溶剂体系,确定了以乙酸乙酯-正丁醇-1.5%氨水(1:4:5,V/V/V)为HSCCC的两相溶剂体系,并运用此溶剂体系,上相为固定相,下相为流动相,主机转速850r/min,流动相流速为1.5m L/min,检测波长为254nm条件下进行分离制备,在250min内从200mg蛹虫草子实体粗提物中一步分离得到10.8mg纯度99%的虫草素和6.1mg纯度98%的N6-(2-羟乙基)-腺苷。该方法简便、快速,为虫草素和N6-(2-羟乙基)-腺苷的大量制备建立了基础。  相似文献   

5.
目的 研究丹酚酸B对离体大鼠工作心脏血流动力学的影响.方法 采用Langendorff离体心脏灌流的方法,以左室内压( LVSP)、左室舒末压(LVEDP)、室内压最大上升速率(+dp/dtmax)、室内压最大下降速率(- dp/dtmax)、心率(HR)等血流动力学参数为指标,观察丹酚酸B对心肌收缩性能的影响.结果 不同剂量(10、5、2.5 mg/L)的丹酚酸B可使LVSP、±dp/dtmax明显升高,同时使HR减慢,并呈剂量依赖性,但对LVEDP无明显作用.结论 丹酚酸B对离体工作心脏有剂量依赖性正性肌力作用.  相似文献   

6.
建立了同时提取丹参中丹参酮ⅡA与丹酚酸B两种主要活性成分的方法及丹酚酸B的纯化工艺。以丹参酮ⅡA与丹酚酸B的含量为评价指标,采用正交实验优化提取工艺,所得最优提取工艺为:用8倍量70%乙醇回流提取3次,每次1 h。丹参酮ⅡA的提取率在90%以上,丹酚酸B的提取率在80%以上。提取物浸膏用热水溶解,过滤,滤液浓缩为1 m L含约0.5 g生药的溶液,取150 m L以2 BV/h的速度上D101大孔树脂柱;然后用6 BV的水洗脱,再以4 BV/h的流速用8 BV的30%乙醇洗脱除杂,以2 BV/h的流速10 BV60%乙醇富集,得到纯度大于75%丹酚酸B,验证实验表明该工艺稳定可行;最后经过洗涤和甲醇重结晶,得到纯度大于99%的丹酚酸B,总得率为2.86%(以干燥根茎计算)。  相似文献   

7.
应用高速逆流色谱法首次从花生壳中分离制备了3种黄酮类化合物。以正己烷-乙酸乙酯-甲醇-水-冰醋酸(5:3:3.5:5:0.25,v/v)为两相溶剂系统,在主机转速800 r/min、流速2 mL/min、检测波长275 nm条件下进行分离制备,纯度用HPLC法测定,各化合物结构经质谱和核磁共振氢谱、碳谱鉴定。结果表明,100 min内从70 mg花生壳粗提物中一步分离制备得到木犀草素11.0 mg,香叶木素2.2 mg,5,7-二羟基色原酮5.2 mg,其纯度均达96.0%以上。利用该方法可以对花生壳中的黄酮类化合物进行快速的分离和纯化。  相似文献   

8.
采用聚酰胺色谱结合高速逆流色谱法分离纯化了萹蓄中3种黄酮类化合物,建立了快速分离制备萹蓄中3种黄酮类化合物的方法。通过聚酰胺柱色谱富集黄酮类成分,再经过高速逆流色谱分离,以乙酸乙酯-甲醇-水-甲酸(体积比为4∶1∶5∶0.1)组成的二相系统作为固定相与流动相,在主机转速为850 rpm,流速为2.0m L/min,检测波长为254 nm的条件下制备样品。从150 mg富集黄酮成分的馏分中,一次性分离制备得到纯度为94.86%的杨梅树皮苷(myricitrin)7.5 mg,94.28%的黄芪苷(astragalin)13.8 mg,91.86%的合欢草素1(desmanthin-1)20.6 mg。所得馏分经高效液相色谱法(HPLC)检测纯度,并经MS和NMR鉴定化合物的结构。该方法简便、快速,所得产物纯度高,适合于黄酮类化合物的制备分离。  相似文献   

9.
本实验建立一种快速从灵芝子实体中制备灵芝烯酸B的方法。以沪农灵芝1号子实体乙醇提取物为原料,经过D101大孔树脂粗分,用60%乙醇洗脱后,采用高速逆流色谱对获得的灵芝酸性三萜进行分离制备。确定最佳溶剂体系为正己烷-乙酸乙酯-甲醇-水(V/V/V/V,5:5:2:9),上相作为固定相,下相作为流动相,单因素法和正交实验设计确定高速逆流色谱法分离灵芝烯酸B的最佳工艺为:流速2.0mL/min,转速900r/min,一次上样量为500mg时,制备得到灵芝烯酸B化合物得率为(9.07±0.16)%,纯度为(85.04±3.45)%。用质谱、核磁对得到的灵芝烯酸B进行了结构鉴定。此法操作简单高效,为大量制备灵芝烯酸B提供了参考。  相似文献   

10.
为比较不同来源的丹参(Salvia miltiorrhiza)药材的酚酸类成分,采用化学指纹图谱和定量分析的方法,对不同来源丹参药材中的酚酸类成分进行了系统分析。结果表明:产地、采收期、病害、根色、根的粗细以及药材部位等因素尽管对丹参酚酸类成分绝对含量的影响比较大,但对各成分相对含量的影响较小;不同来源丹参药材酚酸类成分指纹图谱相似性较高;8月份采收的药材,丹酚酸B含量较高;病害能够显著降低丹酚酸B的积累;与白根和褐色根相比,砖红色根中的丹酚酸B含量较高;根越粗,丹酚酸B含量也越高。这为丹参药材的品质评价和资源利用提供了依据。  相似文献   

11.
A method for extraction and preparative separation of tanshinones from Salvia miltiorrhiza Bunge was successfully established in this paper. Tanshinones from Salvia miltiorrhiza Bunge were extracted using ethyl acetate as the extractant under reflux. The extracts were then purified by high speed counter-current chromatography (HSCCC) with light petroleum-ethyl acetate-methanol-water (6:4:6.5:3.5, v/v) as the two phase solvent system. The upper phase was used as the stationary phase and the lower phase as the mobile phase. 8.2mg of dihydrotanshinone I, 5.8 mg of 1,2,15,16-tetrahydrotanshiquinone, 26.3mg of cryptotanshinone, 16.2mg of tanshinone I, 25.6 mg of neo-przewaquinone A, 68.8 mg of tanshinone IIA and 9.3mg of miltirone were obtained from 400mg of extracts from Salvia miltiorrhiza Bunge in one-step HSCCC separation, with the purity of 97. 6%, 95.1%, 99.0%, 99.1%, 93.2%, 99.3% and 98.7%, respectively, as determined by HPLC area normalization method. Their chemical structures were identified by 1H NMR.  相似文献   

12.
高速逆流色谱用于天然产物分离和指纹图谱构建   总被引:17,自引:0,他引:17  
利用国产高速逆流色谱分离纯化雪莲黄酮类成分和丹参醌类成分。雪莲分离选用氯仿 甲醇 水 (10∶7∶3)体系 ,固定相保留率 72 % ,仪器参数 80 0r min 2mL min ,采用一步洗脱法 ,7h内得到 14个组分 ;丹参分离选用正己烷 乙醇 水 (10∶5 5∶4 5 )体系 ,固定相保留率达到 78 8% ,采用分步洗脱 ,3个产地丹参在 13h内各分离得到 12个洗脱组分。HSCCC洗脱图谱可以表现出不同产地丹参的差别 ,并且各对应洗脱峰保留时间的相对标准偏差 <3% ,因此提出将HSCCC作为构建中药指纹图谱的方法之一 ,其可行性需要通过与常规的指纹图谱构建方法比较之后做出评价。  相似文献   

13.
目的:比较丹参注射液与丹参多酚酸盐注射液对不稳定型心绞痛(UA)患者冠状动脉微循环的影响。方法:将2014年5月~2017年5月105例UA患者随机分为丹参组(n=50)与丹参多酚酸盐组(n=55),前者在PCI术前静脉滴注丹参注射液20 mL,1次/d,连续3 d;后者静脉滴注丹参多酚酸盐注射液200 mg,1次/d,连续3 d。分别在PCI术前及术后即刻检测冠状动脉血流储备(CFR)、冠状动脉微循环阻力系数(IMR)及TIMI血流分级。结果:两组术后CFR、IMR及TIMI血流分级均较术前明显改善(P0.05),丹参多酚酸盐组IMR明显小于丹参组(P0.05),CFR、TIMI血流分级与丹参组比较无统计学意义(P0.05)。结论:丹参注射液与丹参多酚酸盐注射液均能显著改善UA患者的冠状动脉微循环,丹参多酚酸盐注射液一定程度上优于丹参注射液。  相似文献   

14.
High-performance liquid chromatographic (HPLC) fingerprints were developed for identification of both lipophilic and hydrophilic components of the roots of Salvia miltiorrhiza and four related preparations. These samples were separated with an Agilent Zorbax Extend C(18) reserved-phase column (5 microm, 250 mm x 4.6 mm) by linear gradient elution using water-phosphoric acid (100:0.026, v/v) and acetonitrile as mobile phase. The flow rate was 0.8 ml/min and the detector wavelength was set at 280 nm. Mean chromatograms and correlation coefficients of samples were calculated by the software "Similarity Evaluation System for Chromatographic Fingerprint of TCM". The correlation coefficients of Danshen and Fufang Danshen tablets (FDT) samples were in the range of 0.352-0.993 and 0.768-0.987, respectively. The correlation coefficients of Compound Danshen dripping pills (CDDP), Danshen injection (DSI) and Xiangdan injection (XDI) samples were higher than 0.928, 0.850 and 0.960, respectively. It was the first time to identify 34 peaks by comparing with standard compounds and using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS(n)) technique. All results indicated that the developed fingerprint assay could be readily utilized as a quality control method for S. miltiorrhiza and its related preparations.  相似文献   

15.
高速逆流色谱法分离纯化丹参并尝试制订中药指纹图谱   总被引:19,自引:0,他引:19  
用国产高速逆流色谱(HSCCC)分离纯化中草药——丹参,选用正己烷乙醇水体系,固定相保留率达到788%。采用分步洗脱,3个产地丹参各分离得到12个洗脱组分,经高效液相色谱仪和紫外光谱仪检测证明3张HSCCC洗脱图谱中对应洗脱峰为同一组分。HSCCC洗脱图谱不包含非共有峰,并且对应洗脱峰保留时间的相对标准偏差RSD<3%,符合国家标准关于制订指纹图谱方法学考察资料的技术参数。因此,HSCCC作为制订指纹图谱的方法之一具有可行性。  相似文献   

16.
Preparative high-speed counter-current chromatography (HSCCC) coupled with evaporative light scattering detection (ELSD) was used to isolate and separate bioactive constituents from the roots of Aconitum coreanum. Two new diterpenoid alkaloid isomers were successfully separated for the first time by HSCCC with an optimized two-phase solvent system composed of ethyl acetate-n-butanol-methanol-2% acetic acid (3.5:1.5:2:4.5, v/v/v/v), 25.4mg of GFT (1) and 18.3mg of GFU (2) were isolated form 1g crude extract in one step HSCCC experiment. The purities of the two new compounds were all over 95% as analyzed by HPLC and their structures were identified by ESI-MS, (1)H NMR, (13)C NMR, and 2D NMR analysis.  相似文献   

17.
The six phenolic constituents are water-soluble components extracted from the Chinese medical herb danshen, the dried roots of Salvia miltiorrhiza Bunge (Labiatae). An liquid chromatography/tandem mass spectrometry (LC/MS/MS)-based method has been developed for the simultaneous quantification of six phenolic constituents of danshen (magnesium lithospermate B (MLB), rosmarinic acid (RA) and lithospermic acid (LA), caffeic acid (CAA), protocatechuic aldehyde (3,4-dihydroxybenzaldehyde, Pal), 3,4-dihydroxyphenyllactic acid (danshensu)) in human serum with chloramphenicol as internal standard. The serum samples were treated by special liquid-liquid extraction, and the analytes were determined using electrospray negative ionization mass spectrometry in the multiple reaction monitoring (MRM) mode, with sufficient sensitivity to allow analysis of human serum samples generated following administration of a clinically relevant dose. Good linearity over the range 8-2048 ng/mL for six phenolic constituents was observed. The intra- and inter-day precisions (CV) of analysis were <13%, and the accuracy ranged from 88 to 116%. This quantitation method was successfully applied to a pharmacokinetic study of i.v. drip infusion of Danshen injection fluid in human.  相似文献   

18.
腐殖酸对丹参生长的促进作用及其机理的研究   总被引:5,自引:0,他引:5  
本文旨在研究腐殖酸对丹参生长的促进作用及其机理以提高丹以的产量和品质。水培试验研究表明:20ppm-80ppm腐殖酸促进了丹参根干物质的积累,80ppm时达到了最大,丹参根重比对照增加了49%,其作用机理是:通过提高根系活力,增加根系吸收能力,促进谷氨酸合成酶的活性、提高氮同化的效率,促进丹参根系分泌酸性磷酸酯酶以及改变体内酸性和中性磷酸酯酶的活性,以充分利用内的磷而适应低磷环境。  相似文献   

19.
An on-line method based upon dynamic microwave-assisted extraction (DMAE) coupled with high-speed counter-current chromatography (HSCCC) was developed for continuous isolation of nevadensin from Lyeicnotus pauciflorus Maxim. The DMAE parameters were optimized by means of the Box-Behnken design. The maximum extraction yield was achieved using 30:1 ml/g of liquid-solid ratio, 10 ml/min of solvent flow rate and 200 W of microwave power. The crude extracts were then separated by HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (7:3:5:5, v/v/v/v). 13.0mg of nevadensin was isolated from 15.0 g original sample by HSCCC with five times sample injection in 12h, and the isolation yield of nevadensin was 0.87 mg/g. The average purity of nevadensin was higher than 98.0%. The chemical structure of collected fraction was identified by HPLC, ESI-MS and (1)H NMR. The results indicated that this on-line method was effective and fast for high-throughput isolation of nevadensin from L. pauciflorus Maxim.  相似文献   

20.
连接有蒸发光散射检测器的高速逆流色谱仪首次成功的应用于制备和分离青葙子中的皂苷celosins A和B.二氯甲烷∶正丁醇∶甲醇∶水(4∶0.3∶3∶2)+0.5%冰醋酸作为洗脱溶剂系统.从半制备型HSCCC收集到的组分进行HPLC分析,可以得到:celosin A纯度为98.9%,celosin B的纯度为98.1%.这是高速逆流色谱仪首次被用于纯化青葙子中的皂苷,两个化合物的结构通过碳谱和质谱来确定.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号