共查询到20条相似文献,搜索用时 15 毫秒
1.
Wei Xin SUN Qiang ZHANG Jian Qin JIANG 《中国化学快报》2006,17(8):1054-1056
Daphne giraldii Nitsche (Thymelaeaceae) is widely distributed in Shanxi, Gansu, Sichuan and Ningxia provinces of China. According to the modern research, it showed the activity against inflammatory, pain, cancer and so on1. Herein we report the identifica… 相似文献
2.
Altertoxin I (ATX I) is one of the common mycotoxins produced by genus Alternaria which is a common food pathogen of fruits and grains. To prepare enough quantity of pure ATX I for further research of mutagenicity and toxicology tests, a novel method using preparative high-speed counter-current chromatography (HSCCC) was developed. The ethyl acetate crude extracts of the acetone washes obtained after fermentation of Alternaria sp. was separated using a two-phase solvent system composed of n-hexane–ethyl acetate–methanol–water (2:5:5:6, v/v). Collected fractions were analyzed by LC and identified by EI–MS and NMR analysis. The technique can isolate mg levels of the target compound per run.
相似文献3.
Dejun Hu Miao Liu Xing Xia Daijie Chen Fengsheng Zhao Mei Ge 《Chromatographia》2008,67(11-12):863-867
Altertoxin I (ATX I) is one of the common mycotoxins produced by genus Alternaria which is a common food pathogen of fruits and grains. To prepare enough quantity of pure ATX I for further research of mutagenicity and toxicology tests, a novel method using preparative high-speed counter-current chromatography (HSCCC) was developed. The ethyl acetate crude extracts of the acetone washes obtained after fermentation of Alternaria sp. was separated using a two-phase solvent system composed of n-hexane–ethyl acetate–methanol–water (2:5:5:6, v/v). Collected fractions were analyzed by LC and identified by EI–MS and NMR analysis. The technique can isolate mg levels of the target compound per run. 相似文献
4.
Su J Wu ZJ Zhang WD Zhang C Li HL Liu RH Shen YH 《Chemical & pharmaceutical bulletin》2008,56(4):589-591
Two new bis-coumarin glycosides were isolated from the stem barks of Daphne giraldii NITSCHE. Their structures were elucidated as 6-O-alpha-L-rhamnnopyranosyl daphnogirin (1), and 6-O-beta-D-apiofuranosyl daphnogirin (2), on the basis of detailed spectroscopic analysis. Compounds 1 and 2 were tested inhibitory effects against production of nitric oxide (NO) in RAW264.7 cells, and cytotoxicity of human tumor cell lines A549, LOVO, QGY-7703, 6T-CEM. The results showed that compounds 1 and 2 neither reduced production of NO, nor inhibited human tumor cell lines. 相似文献
5.
A preparative high-speed countercurrent chromatography (HSCCC) method for isolation and purification of three bioactive components, tectoquinone; 1-hydroxy-2-methylanthraquinone and mollugin from the Chinese medicinal plant Rubia cordifolia was successfully established. With a two-phase solvent system composed of light petroleum/ethanol/diethyl ether/water (5:4:3:1, v/v), 10 mg tectoquinone, 19 mg 1-hydroxy-2-methylanthraquinone and 16 mg mollugin were obtained from 100 mg of the crude petroleum extract in a one-step separation at a purity of 98.8, 95.8 and 98.3%, respectively. The structures of mollugin and anthraquinones were identified by 1H NMR and 13C NMR. 相似文献
6.
Two new bis‐coumarins, namely daphnogitin ( 1 ), daphnogirin ( 2 ), and a flavan‐3‐ol derivative, 5‐O‐methylafzelechin ( 3 ), together with eleven known compounds, daphnetoxin, 1,2‐dihydrodaphnetoxin, daphnetin, daphnoretin, daphneticin, isodaphneticin, trans‐2,3‐dihydro‐3‐(4‐hydroxy‐3‐methoxyphenyl)‐2‐(hydroxymethyl)‐9H‐pyrano[2,3‐f]‐1,4‐benzodioxin‐9‐one (= demethoxyisodaphneticin; 4b ), (+)‐pinoresinol, acuminatin, (−)‐dihydrosesamin, and isosalicifoline, were isolated from the leaves and stems of Daphne giraldii. Compound 4b was isolated for the first time as a natural product, and 1,2‐dihydrodaphnetoxin, daphneticin, isodaphneticin, (+)‐pinoresinol, acuminatin, (−)‐dihydrosesamin, and isosalicifoline were isolated for the first time from Daphne giraldii. The structures of the three new compounds were elucidated by spectroscopic analysis. 相似文献
7.
Juan Su Zhi Jun Wu Run Hui Liu Yun Heng Shen Chuan Zhang Hui Liang Li Wei Zhang Wei Dong Zhang 《中国化学快报》2007,18(7):835-836
A new coumarin glycoside was isolated from the ethanol extract of the barks of stem of Daphne giraldii Nitsche. Its structure was defined as daphnetin 8-O-b-D-glucopyranosyl-(1→6)-b-D-glucopyranoside on the basis of spectral evidences. 相似文献
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Nisar Ullah Prinz Sonja Ernst Haslinger Wagar Ahmed Mohammed Arfan Abdul Malik 《Helvetica chimica acta》2001,84(1):157-162
Three new natural products, a lignoid glycoside 1 and two dimeric phenylpropanoids 2 and 3 , along with two known lignans 4 and 5 , were isolated from the BuOH‐ and CHCl3‐soluble fractions of the whole plant of Daphne oleoides (Thymelaeaceae). The structures of the new compounds were established by spectroscopic techniques, including 2D NMR, as 4‐(β‐D ‐glucopyranosyloxy)‐9′‐hydroxy‐3,3′,4′‐trimethoxy‐7′,9‐epoxylignan ( 1 ), (1R,2S,5R,6R)‐6‐(3‐ethyl‐4‐hydroxy‐5‐methoxyphenyl)‐2‐(4‐hydroxy‐3,5‐dimethoxyphenyl)‐3,7‐dioxabicyclo[3.3.0]octane ( 2 ) and (1R,2S,5R,6S)‐2,6‐bis(3‐ethyl‐4‐hydroxy‐5‐methoxyphenyl)‐3,7‐dioxabicyclo[3.3.0]octane ( 3 ). The other lignans were identified as (+)‐pinoresinol O‐(β‐D ‐glucopyranoside) ( 4 ) and (+)‐medioresinol ( 5 ). 相似文献
10.
芦荟色酮的高速逆流色谱分离制备方法研究 总被引:12,自引:0,他引:12
芦荟色酮是在芦荟叶中特有的一类具有抗炎和抑制酪氨酸酶等作用的活性物质。以芦荟全叶为原料,经过一系列的预处理手段,从脱色剂活性炭中获得芦荟色酮粗提物,再经过溶剂分配和富集后采用高速逆流色谱(HSCCC)对其中的色酮成分进行分离纯化。研究结果表明,采用氯仿-甲醇-水(体积比为4∶3∶2)混合溶液和二氯甲烷-甲醇-水(体积比为5∶4∶2)混合溶液作为溶剂分离系统,经过两步HSCCC可以分离纯化出色谱纯度在95%以上的芦荟色酮单体。经过紫外检测、快原子轰击质谱及核磁共振等方法的结构分析鉴定,证实分离所得物质为肉桂酰基-C-葡萄糖甙芦荟色酮。 相似文献
11.
Zhou GX Jiang RW Cheng Y Ye WC Shi JG Gong NB Lu Y 《Chemical & pharmaceutical bulletin》2007,55(9):1287-1290
Two new biflavonoids, daphnogirins A (1) and B (2), were obtained from the roots of Daphne giraldii. Their structures were established on the basis of the spectral data and X-ray diffraction data of the co-crystal of 1 and 2. Daphnogrins A and B have the same configuration at C-1 and opposite configurations at C-16 and C-17. Oxygen radical scavenging assay has indicated that they are of significant antioxidative activity. 相似文献
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高速逆流色谱法分离纯化黄芪中的芒柄花素和毛蕊异黄酮 总被引:19,自引:0,他引:19
采用高速逆流色谱法(HSCCC),以正己烷-氯仿-甲醇-水组成二相系统作为固定相与流动相,对黄芪的乙酸乙酯粗提
物进行了分离纯化。 结果发现:以正己烷-氯仿-甲醇-水(体积比为1.5∶3∶3∶2)组成的系统可以从黄芪的乙酸乙酯粗
提物中分离出毛蕊异黄酮,纯度可达95%以上,并可以初步纯化芒柄花素;接着用正己烷-氯仿-甲醇-水(体积比为4∶4∶5
∶4)组成的系统进一步纯化芒柄花素,其纯度达95%以上。利用该方法,可以对中药黄芪中的异黄酮进行快速的分离和纯
化。 相似文献
14.
An efficient and simple method to isolate and purify highly polar antioxidants from the antioxidant active site of Chirita longgangensishas been established. Firstly, the antioxidant active site was enriched with D101 macroporous resin, and then high-speed counter-current chromatography (HSCCC) was used with the two-phase solvent system ethyl acetate–n-butanol–methanol–water (5:0.1:0.5:4.5, v/v) to obtain four antioxidants in one step. They were identified as plantainoside D (28.4 mg), plantainoside B (9.5 mg), calcedarioside B (18.1 mg) and calcedarioside A (16.7 mg) by analysis of electrospray ionization mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR) spectra. The purities were all above 97 % as determined by HPLC. The inhibiting effects of the crude extracts, enriched fraction and the obtained compounds on superoxide anion radical, hydroxyl radical and hydrogen peroxide were determined by different chemiluminescence (CL) systems. The result shows that all of them have good antioxidant activity. However, the sequence of antioxidant abilities among compounds I–IV was different when assayed by different CL systems (superoxide anion radical, hydroxyl radical, and hydrogen peroxide). This is the first report on preparative isolation and purification of antioxidants from C. longgangensis by HSCCC combined with macroporous resin and their inhibition of free radical-induced luminol chemiluminescence. 相似文献
15.
反相制备液相色谱分离白花败酱草异戊烯基黄酮 总被引:3,自引:1,他引:3
用半制备型反相高效液相色谱(RPLC)对白花败酱草氯仿萃取物进行了分离制备。色谱柱为YWGC18(200 mm×10.0 mm i.d.,10μm),流动相为乙腈∶水∶乙酸(55∶45∶1,V/V),检测波长280 nm,流速4.0mL/m in,进样750μL(样品液浓度30 g/L)。在此条件下一次分离得到5个单体化合物,经理化反应和光谱分析分别鉴定为bolusanthol B(1),(2S)-5,7,2,′6-t′etrahydroxy-6-lavandu lylated flavanone(2),(2S)-5,2,′6-′trihydroxy-2,″2-″d im ethylpyrano[5,″6″∶6,7]flavanone(3),orotin in(4)和orotin in-5-m ethyl ether(5)。其中2和3为新化合物,1、4和5为首次从败酱属植物中分离得到。 相似文献
16.
Simultaneous determination and pharmacokinetic study of giraldoid a,giraldoid B in rat plasma after oral administration of Daphne giraldii Nitsche extracts by LC–MS/MS 下载免费PDF全文
《Biomedical chromatography : BMC》2018,32(3)
A simple sensitive LC–MS/MS method has been developed for the simultaneous determination of giraldoid A and giraldoid B in rat plasma. The method was applied to pharmacokinetics studies of the two compounds from Daphne giraldii Nitsche. Chromatographic separation was accomplished on an Acquity UPLC™ BEH C18 column (100 × 2.1 mm, 1.7 mm) by gradient elution with a flow rate of 0.2 mL min−1. The method was linear over the concentration range of 1.0–1000 ng mL−1, and the lower limits of quantification were 1.04 ± 0.10 and 1.04 ± 0.09 ng mL−1, respectively. The intra‐ and inter‐day precisions (RSD) were <10.14 and 9.96%. The extraction recovery of the analytes was acceptable. Stability studies demonstrated that the two compounds were stable in the preparation and analytical process. The maximum plasma concentration was 687.78 ± 243.62 ng mL−1 for giraldoid A and 952.38 ± 131.99 ng mL−1 for giraldoid B. The time to reach the maximum plasma concentration was 0.50 ± 0.37 h for giraldoid A and 0.50 ± 0.66 h for giraldoid B. The validated method was successfully applied to investigate the concentration–time profiles of giraldoid A and giraldoid B. 相似文献
17.
Petr Marhol Petr Bednář Eva Tománková Barbora Papoušková Jan Stávek Pavel Híc Petr Barták Vladimír Křen Josef Balík 《Chromatographia》2013,76(17-18):1107-1115
Untreated silica gel was used as the stationary phase for a simple and cost-effective prepurification of 5-carboxypyranoanthocyanins from red wine enriched by the addition of pyruvic acid. The composition of the fractions obtained was analyzed by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC/MS2) and the results enabled the changes in 5-carboxypyranoanthocyanin profile during preparative separation to be described and explained. Repeated purification on silica gel followed by reversed-phase separation enabled the isolation of 5-carboxypyranomalvidin-3-glucoside in high purity and represents a cheap and robust alternative to the commonly used procedures. Reversed-phase preparative chromatography with an isocratic elution [15 % acetonitrile in water (v/v)] provided sufficient resolution, showing that the addition of an acid is not necessary in anthocyanin separation. The antioxidant capacity of 5-carboxypyranomalvidin-3-glucoside was compared with malvidin-3-glucoside and a group of common polyphenols (e.g., gallic acid, quercetin, rutin, and catechin). 相似文献
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Yi Yang Yun Huang Dongyu Gu Abulimiti Yili Gulnar Sabir Haji Akber Aisa 《Chromatographia》2009,69(9-10):963-967
Following an initial clean-up step on a Sephadex LH-20 column, high-speed countercurrent chromatography was successfully applied to the isolation and purification of three flavonoids from a crude sample of Helichrysum arenarium (L.) Moench. HSCCC was performed with a two-phase solvent system composed of ethyl acetate–water (1:1, v/v). Naringenin-7-O-β-d-glycoside (2.3 mg), isoquercitrin (3.5 mg), and astragalin (6.7 mg), with purities of 96.05%, 93.63%, 95.23%, respectively, were separated from 160 mg of crude sample in a one-step separation. The structure identification was by 1H NMR and 13C NMR. 相似文献
20.
《液相色谱法及相关技术杂志》2012,35(15):3297-3309
Abstract The chiral stationary phases (CSP's) that have proceeded from the work of Dr. Pirkle of the University of Illinois have characteristics especially useful to preparative liquid chromatography: Packings made with such CSP's can be highly efficient, lose efficiency only gradually when overloaded and regain it immediately when overload is removed, and allow the elution order of enantiomers to be reversed. These have been used at Regis in both preparative and analytical chromatography: in demonstration, to purify an enantiomer to 99.9967% optical purity and to determine that degree of optical purity with adequate precision and sensitivity. Both the relevant theory and the experimental work suggest that preparative trace-first chromatography is eminently suited to purification to high degree, and becoming the better suited as the degree of purity increases. 相似文献