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 46 毫秒
1.
Lu Y  Sun C  Wang Y  Pan Y 《Journal of chromatography. A》2005,1089(1-2):258-262
Two phenylbutenoids, (E)-4-(3',4'-dimethoxyphenyl)but-3-enyl acetate and (E)-4-(3',4'-dimethoxyphenyl)but-1,3-diene, were separated from the rhizomes of Zingiber Cassumunar using a preparative upright counter-current chromatography (CCC). With a two-phase solvent system composed of light petroleum (b.p. 60-90 degrees C)-ethanol-diethyl ether-water (5:4:2:1, v/v), 150 mg of (E)-4-(3',4'-dimethoxyphenyl)but-3-enyl acetate and 175 mg of (E)-4-(3','-dimethoxyphenyl)but- 1,3-diene with the purity of 98.7 and 95.1%, respectively, were obtained from 600 mg of the crude sample of Z. Cassumunar in a single-step separation. Structures of these two compounds were identified by ESI-MS, 1H NMR and 13C NMR.  相似文献   

2.
Wang X  Geng Y  Li F  Shi X  Liu J 《Journal of chromatography. A》2006,1115(1-2):267-270
pH-zone-refining counter-current chromatography was successfully applied to the separation of alkaloids from a crude extract of Corydalis decumbens (Thunb.) Pers. using a multilayer coil planet centrifuge (CPC). The experiment was performed with a two-phase solvent system composed of methyl tert-butyl ether (MtBE)-acetonitrile-water (2:2:3, v/v) where triethylamine (5-10 mM) was added to the upper organic stationary phase as a retainer and hydrochloric acid (5-10 mM) to the aqueous mobile phase as an eluter. From 3.1 g of the crude extract, 495 mg protopine, 626 mg tetrahydropalmatine and 423 mg bicuculline were obtained each with a purity of over 93% as determined by high performance liquid chromatography. The structures of the isolated compounds were identified by electron ionization mass spectrometry (EI-MS), high-performance liquid chromatography (HPLC)-electrospray ionisation-mass spectrometry (ESI-MS) and 1H NMR.  相似文献   

3.
Preparative high-speed counter-current chromatography (HSCCC) coupled with evaporative light scattering detection (ELSD) was employed for the isolation and purification of alkaloids from the roots of Aconitum coreanum (Lèvl.) Rapaics. The two-phase solvent system used in HSCCC was n-hexane-ethyl acetate-methanol-0.2M HCl (1:3.5:2:4.5, v/v/v/v). Six alkaloids were obtained and yielded 10.4 mg of Guanfu base P, 9.2 mg of Guanfu base G, 9.5 mg of Guanfu base F, 8.9 mg of atisine, 11.9 mg of Guanfu base A and 25.7 mg of Guanfu base I from 2 g of crude extracts. The purity of these compounds was 96.9%, 95.7%, 91.5%, 98.9%, 95.8% and 95.5%, respectively, as determined by high-performance liquid chromatography (HPLC). Their chemical structures were identified by MS, (1)H NMR and (13)C NMR.  相似文献   

4.
pH‐zone‐refining centrifugal partition chromatography was successively applied in the large‐scale separation of close Rf antipsychotic indole alkaloids directly from CHCl3 fraction of Rauwolfia tetraphylla leaves. Two experiments with increasing mass from 500 mg to 3 g of crude alkaloid extracts ( 1 C) of R. tetraphylla were carried out in normal‐displacement mode using a two‐phase solvent system composed of methyl tert‐butyl ether/ACN/water (4:1:5, v/v/v) where HCl (12 mM) was added to the lower aqueous stationary phase as a retainer and triethylamine (5 mM) to the organic mobile phase as an eluter. The two centrifugal partition chromatography separations afforded a total of 162.6 mg of 10‐methoxytetrahydroalstonine ( 1 ) and 296.5 mg of isoreserpiline ( 2 ) in 97% and 95.5% purity, respectively, along with a 400.9 mg mixture of α‐yohimbine and reserpiline ( 3 and 4 ). Further, this mixture was resolved over medium pressure LC using TLC grade silica gel H (average particle size 10 μm), which afforded 160.4 mg of α‐yohimbine ( 3) and 150.2 mg of reserpiline ( 4) in >95% purities. The purity of the isolated antipsychotic alkaloids was analyzed by high‐performance LC and their structures were characterized on the basis of their 1D, 2D NMR and electrospray ionization‐mass spectroscopic data.  相似文献   

5.
Jiang L  Lu Y  He S  Pan Y  Sun C  Wu T 《Journal of separation science》2008,31(22):3930-3935
High-speed counter-current chromatography (HSCCC) was applied to the preparative isolation and purification of two amides from Mallotus lianus Croiz. In a single HSCCC separation, using the two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (5:1:5:1 v/v), 247.5 mg of the enriched crude sample was separated to afford 10.3 mg of N-isobutyl-2E,4E,12Z-octadecatrienamide and 15.7 mg of (7Z,10Z,18Z)tricosa-7,10,18-trienamide, a novel compound, with the purities of 98.0 and 94.6%, respectively. The HSCCC fractions were analyzed by HPLC and chemical structures of the compounds were identified by 1D- and 2D-NMR, ESI-, and GC-MS.  相似文献   

6.
An effective high‐speed countercurrent chromatography method was successfully established by using ionic liquids as the modifier of the two‐phase solvent system. Adding a small amount of ionic liquids significantly shortens the separation time and improves the separation efficiency. The conditions of ionic‐liquid‐modified high‐speed countercurrent chromatography including solvent systems, types and content of added ionic liquids, and ionic liquids posttreatment were investigated. The established method was successfully applied to separate alkaloids from lotus leaves using a two‐phase solvent system composed of petroleum ether/ethyl acetate/methanol/water/[C4mim][BF4] (1:5:1:5:0.15, v/v/v/v/v). Four alkaloids pronuciferine (1.7 mg), N‐nornuciferine (4.3 mg), nuciferine (3.1 mg), and roemerine (2.1 mg) were obtained with the purities of 90.53, 92.25, 99.86, and 98.63%, respectively, from 100 mg crude extract of lotus leaves. The results indicated that the ionic‐liquid‐modified high‐speed countercurrent chromatography method was suitable for alkaloid separation from lotus leaves and would be a promising method for the separation of alkaloids from other natural products.  相似文献   

7.
Liu M  Zhang S  Yang C  Xia Y  Liu J  Liang J 《色谱》2011,29(5):430-434
应用高速逆流色谱法分离制备了生附子中的3个C19型二萜生物碱类化合物。以正己烷-乙酸乙酯-甲醇-水(3:5:4:5, v/v/v/v)为两相溶剂系统,上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2.0 mL/min、检测波长235 nm条件下进行分离制备;一次性从90 mg附子总碱粗提物中分离制备得到15.3 mg北草乌碱,35.1 mg中乌头碱和22.7 mg次乌头碱,经高效液相色谱分析,测得它们的纯度分别为97.9%、96.2%和99.2%。并应用波谱(电喷雾离子质谱、核磁共振氢谱和核磁共振13C谱)解析法确定了它们的结构。利用该方法可以对生附子中的二萜类生物碱成分进行快速的分离和纯化  相似文献   

8.
C19‐diterpenoid alkaloids are the main components of Aconitum duclouxii Levl. The process of separation and purification of these compounds in previous studies was tedious and time consuming, requiring multiple chromatographic steps, thus resulted in low recovery and high cost. In the present work, five C19‐diterpenoid alkaloids, namely, benzoylaconine ( 1 ), N‐deethylaconitine ( 2 ), aconitine ( 3 ), deoxyaconitine ( 4 ), and ducloudine A ( 5 ), were efficiently prepared from A. duclouxii Levl (Aconitum L.) by ethyl acetate extraction followed with counter‐current chromatography. In the process of separation, the critical conditions of counter‐current chromatography were optimized. The two‐phase solvent system composed of n‐hexane/ethyl acetate/methanol/water/NH3·H2O (25%) (1:1:1:1:0.1, v/v) was selected and 148.2 mg of 1 , 24.1 mg of 2 , 250.6 mg of 3 , 73.9 mg of 4, and 31.4 mg of 5 were obtained from 1 g total Aconitum alkaloids extract, respectively, in a single run within 4 h. Their purities were found to be 98.4, 97.2, 98.2, 96.8, and 96.6%, respectively, by ultra‐high performance liquid chromatography analysis. The presented separation and purification method was simple, fast, and efficient, and the obtained highly pure alkaloids are suitable for biochemical and toxicological investigation.  相似文献   

9.
Niu L  Xie Z  Cai T  Wu P  Xue P  Chen X  Wu Z  Ito Y  Li F  Yang F 《Journal of separation science》2011,34(9):987-994
High‐speed counter‐current chromatography (HSCCC) was successfully applied for the preparative separation and purification of alkaloids from Corydalis bungeana Turcz. (Kudiding in Chinese) for the first time. After the measurement of partition coefficient of seven target alkaloids in the nine two‐phase solvent systems composed of CHCl3–MeOH–(0.1 M; 0.2 M; 0.3 M) HCl (4:1.5:2; 4:2:2; 4:3:2, v/v), CHCl3–MeOH–0.2 M HCl (4:2:2, v/v) and CHCl3–MeOH–0.3 M HCl (4:3:2, v/v) were finally selected for the HSCCC separation using the first upper phase as the stationary phase and the stepwise elution of the two lower mobile phases. Consequently, sanguinarine (10 mg), corynoline (25 mg), protopine (20 mg), corynoloxine (18 mg), and 12‐hydroxycorynoline (8 mg) were obtained from 200 mg of crude alkaloid extracts with purities of 94–99% as determined by HPLC. Their chemical structures were characterized on the basis of 1H‐NMR, 13C‐NMR, and LC‐ESI‐Q‐TOF‐MS/MS analyses.  相似文献   

10.
Preparative high-speed counter-current chromatography (HSCCC) was successfully used for isolation and purification of trans-3,5,4'-trihydroxystilbene-4'-O-beta-D-glucopyranoside (compound 1) and (+)catechin (compound 2) from Rheum tanguticum Maxim. ex Balf. by stepwise elution with a pair of two-phase solvent system composed of ethyl acetate-ethanol-water (25:1:25, v/v) and (5:1:5, v/v), and stepwise increasing the flow-rate of the mobile phase from 0.8 to 2.0 mlmin(-1) after 5 h. The preparative HSCCC separation was performed on 250 mg of crude extract yielding pure compound 1 (10.2 mg) and compound 2 (26.7 mg) all at purities of over 96% in a single run. The structures of the two compounds have been elucidated by means of spectroscopic methods including MS and 1H, 13C nuclear magnetic resonance spectroscopy.  相似文献   

11.
This paper describes how high-performance counter-current chromatography (HPCCC) was used strategically for the separation of Tripterygium wilfordii Hook. f. Due to the complexity of Chinese herbal medicines, the initial ethanol crude extract was fractionated into seven fractions using medium-pressure liquid chromatography (MPLC). One terpenoid (triptolide) and three alkaloids (peritassine A, wilforgine and wilforine) were further separated from one of the MPLC fractions. This fraction (1.25 g) yielded 8 mg of triptolide and 28 mg of peritassines A after one HPCCC column pass and 30 mg of wilforgine and 120 mg of wilforine after a second column pass with respective purities of 97%, 93.6%, 95.0% and 94.4%, which were determined by high-performance liquid chromatography (HPLC). This was a one-step HPCCC separation, using an n-hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) solvent system, where increases in theoretical plates have been sacrificed in favour of increasing throughput. Structures were identified by electrospray ionization mass spectrometry (ESI-MS), (1)H nuclear magnetic resonance ((1)H NMR) and (13)C nuclear magnetic resonance ((13)C NMR). Comparison of three different modes of eluting compounds retained in the liquid stationary phase: elution extrusion; dual mode and simple pump-out showed that simply pumping out the column contents at high flow gave better resolution and was eight times faster than the other two well-utilised methods. Triptolide and peritassines A were isolated for the first time from Tripterygium wilfordii Hook. f.  相似文献   

12.
A preparative high‐speed counter‐current chromatography method for separation and purification of liensinine, isoliensinine and neferine from seed embryo of Nelumbo nucifera GAERTN was successfully established by using n‐hexane‐ethyl acetate‐methanol‐water (5:8:4:5, v/v, containing 0.5% NH4OH) as the two‐phase solvent system. From 200 mg of crude extract, 18.4 mg of liensinine, 19.6 mg of isoliensinine and 58.4 mg of neferine were obtained with the purity of 96.8, 95.9, and 98.6%, respectively. The identification of the three alkaloids was performed with 1H NMR and 13C NMR.  相似文献   

13.
Supercritical fluid extraction (SFE) was used to extract quinolizidine alkaloids from Sophora flavescens Ait. (Kushen). An orthogonal test L(9)(3)(4) including pressure, temperature, flow rate of CO(2) and the amount of modifier was performed to get the optimal conditions. The process was then scaled up by 30 times with a preparative SFE system under 25 MPa, 50 degrees C and a flow rate of CO(2) (2l/min) and the amount of modifier (0.04 ml/min). The crude extracts were separated and purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of chloroform-methanol-2.3 x 10(-2)M NaH(2)PO(4) (27.5:20:12.5, v/v), and the collected fractions were analyzed by high-performance liquid chromatography (HPLC). Three kinds of quinolizidine alkaloids were obtained, yielding 10.02 mg of matrine, 22.07 mg of oxysophocarpine and 79.93 mg of oxymatrine with purities of 95.6, 95.8, 99.6% in one-step separation, respectively.  相似文献   

14.
Dioscin derivatives from the Dioscorea villosa roots were isolated and purified by centrifugal partition chromatography coupled with evaporative light scattering detection. The two-phase solvent system composed of chloroform-methanol-isopropanol-water (7:6:1:4, v/v/v/v) was used to obtain prosapogenin A of dioscin (1, 11.1 mg), dioscin (2, 8.9 mg), deltonin (3, 29.2 mg) and diosgenin 3-O-[alpha-L-rhamnopyranosyl(1 --> 2)]-[beta-D-glucopyranosyl(1 --> 3)-beta-D-glucopyranosyl(1 --> 4)]-beta-D-glucopyranoside (4, 6.2 mg) from 300 mg of saponin-rich extract from the roots of D. villosa. The purities of 1, 2, 3 and 4 were determined to be 98.9, 97.4, 99.2 and 99.5%, respectively. Their chemical structures were determined by spectroscopic data of ESI-MS, 1H NMR and 13C NMR and comparing with those of previously reported values.  相似文献   

15.
The first preparative separation of two benzoxazinoids, (2R)-2-O-beta-d-glucopyranosyl-2H-1,4-benzoxazin-3(4H)-one (HBOA-Glc) and (2R)-2-O-beta-d-glucopyranosyl-4-hydroxy-2H-1,4-benzoxazin-3(4H)-one (DIBOA-Glc), by means of high-speed counter-current chromatography (HSCCC) from the n-butanol extract of Acanthus ilicifolius L. is presented. The two-phase solvent system containing ethyl acetate-n-butanol-0.5%NH(4)OH (2:3:5, v/v/v, system B) was selected for the one-step HSCCC separation of HBOA-Glc and DIBOA-Glc according to the partition coefficient values (K) for target compounds and the separation factor (alpha) between the two target compounds. In the one-step HSCCC separation using solvent B, from 100mg n-butanol extract of A. ilicifolius, 6.3 mg HBOA-Glc and 6.8 mg DIBOA-Glc were isolated with purities of 90.3% and 80.2%, respectively. In order to obtain the two target compounds with higher purity, a second separation process was developed comprising two steps. In the two-step separation, the sample was first pre-purified by HSCCC using ethyl acetate-n-butanol-water (2:3:5, v/v/v, system A) solvent system and then purified using solvent system B. A 100-mg amount of the n-butanol extracts of A. ilicifolius was separated to yield 5.8 mg of HBOA-Glc and 4.8 mg of DIBOA-Glc with purities of 97.1% and 94.8%, respectively, which were directly used for NMR analyses.  相似文献   

16.
It is known that when methanol extract of Evodia fruit is orally administered, 5-(1,4-dihydro-1-methyl-4-oxo-2-quinolin-2-yl) pentanoic acid (EVCA) is excreated as a matabolite in rat urine. In this study, we separated Evodia fruit extract into major alkaloids administered each alkaloid individually to male Wistar rats. Consequently, it was demonstrated that the original substance of the metabolite are evocarpine and its analogues, dihydroevocarpine and 1-methyl-2-undecenyl-4(1H)-quinolone. Investigation of a blood sample after oral administration of evocarpine by high performance liquid chromatography confirmed that the substance was absorbed without alteration. Pharmacokinetics of evocarpine after intravenous injection was expressed in a one-compartment model, showing a linear elimination of plasma evocarpine up to a dosage of 75 mg/kg. Total plasma clearance (CL), volume of distribution (Vd), and half-life (T1/2) of evocarpine were 60 ml/min.kg, 3.21/kg and 0.6 h-1, respectively. Metabolic ratio of evocarpine into EVCA after intravenous injection was 15.4%, and absorption ratio of the unaltered compound calculated from the levels of AUC after oral administration and intravenous injection was 4.7%. In this paper, it is shown that evocarpine is absorbed amount 100% when it is administered orally.  相似文献   

17.
A preparative high-speed counter-current chromatography (HSCCC) method for isolation and purification of coumarin compounds from the Chinese medicinal plant Peucedanum decursivum (Miq.) Maxim (Zihuaqianhu in Chinese) was successfully established by using light petroleum-ethyl acetate-methanol-water (5:5:7:4, v/v) as the two-phase solvent system. The upper phase of light petroleum-ethyl acetate-methanol-water (5:5:7:4, v/v) was used as the stationary phase of HSCCC. Nodakenetin (2.8 mg), 6.1 mg of Pd-C-IV, 7.3 mg of Pd-D-V, 4.7 mg of ostruthin, 7.8 mg of decursidin and 11.2 mg of decursitin C with the purity of 88.3%, 98.0%, 94.2%, 97.1%, 97.8% and 98.4%, respectively, were separated successfully in one-step separation from 150 mg of crude sample from P. decursivum (Miq.) Maxim. After purified by HSCCC again with light petroleum-ethyl acetate-methanol-water (5:5:4:5, v/v) as the two-phase solvent system, the purity of (I) can reach 99.4%. The structures of all the compounds were identified by 1H NMR and 13C NMR.  相似文献   

18.
(3R)-(-)-7,2'-Dihydroxy-3',4'-dimethyl isoflavan-7-O-beta-D-glucopyranoside and (6aR, 11aR) 9,10-di-methoxypterocarpan-3-O-beta-D-glucopyranoside were separated from the ethyl acetate extract of the root of Astragalus membranaceus Bge. var. mongholicus (Bge.) Hsiao by high-speed counter-current chromatography (HSCCC). A two-phase system composed of ethyl acetate-ethanol-acetic acid-water (4:1:0.25:5, v/v) was selected by analytical HSCCC. Preparative HSCCC yielded, from 100 mg of the partially purified extract, 50 mg of isoflavan glycoside and 10 mg of pterocarpan glycoside each at over 95% purity by high-performance liquid chromatography (HPLC) analysis. Their structures were identified by MS, 1H NMR and 13C NMR.  相似文献   

19.
A preparative high‐speed counter‐current chromatography method for isolation and purification of bufadienolides from ChanSu was developed by using a stepwise elution with two‐phase solvent system composed of n‐hexane/ethyl acetate/methanol/water at the ratios of 4:6:2:4 v/v, 4:6:2.5:4 v/v and 4:6:3.2:4 v/v. A total of 3.8 mg of gamabufotalin (1), 7.2 mg of arenobufagin (2), 3.4 mg of telocinobufagin (3), 5.3 mg of bufotalin (4), 8.5 mg of cinobufotalin (5) and 8 mg of bufalin (6) were obtained in one‐step separation from 80 mg of the crude extract with purity of 92.7, 96.7, 87.2, 97.3, 94.9 and 99.4%, respectively. Their chemical structures were identified on the basis of 1H‐NMR and 13C‐NMR technology.  相似文献   

20.
Following an initial clean-up step on silica, high-speed counter-current chromatography (HSCCC) was used to purify an aryl ketone, 1-[2',4'-dihydroxy-3',5'-di-(3"-methylbut-2"-enyl)-6'-methoxy] phenylethanone from an extract of the stem bark of the shrub Acronychia pedunculata. The two-phase solvent system used was composed of n-heptane-ethyl acetate-methanol-water at an optimized volume ratio of 4:1:4:1 (v/v/v/v). Target compound (58.1 mg) with a purity of 98.9% was obtained after HSCCC of 183.5 mg sample with a purity of 35.7% recovered after the silica clean-up step. Identification of the target compound was performed by 1H NMR, 13C NMR, two-dimensional NMR and LC-electrospray ionization MS.  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