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高速逆流色谱分离纯化防风中升麻素苷和5-O-甲基维斯阿米醇苷 总被引:3,自引:1,他引:2
建立了高速逆流色谱分离制备防风中有效成分升麻素苷和5-O-甲基维斯阿米醇苷的方法.防风根的粉末经甲醇浸泡提取和减压蒸馏,得粗提浸膏.以V(乙酸乙酯):V(正丁醇):V(水)=2:7:9为溶剂,上相为固定相,下相为流动相,流速2.0 mL/min.从316 mg防风粗提物中一步分离得到13.9 mg升麻素苷和25 mg 5-O-甲基维斯阿米醇苷,纯度分别为98.1%和99 2%.采用ESI-MS, 1H NMR 和13C NMR对目标化合物的结构进行了鉴定. 相似文献
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高速逆流色谱法对独角莲中有效成分皂苷的分离纯化 总被引:1,自引:0,他引:1
本文采用高速逆流色谱法对独角莲中的有效成分皂苷进行分离纯化.分别以乙酸乙酯∶正丁醇∶乙腈∶水=5∶1∶1∶5(V/V)及乙酸乙酯∶正丁醇∶乙醇∶水=5∶10∶2∶20(V/V)为溶剂系统,用下相作流动相,上相作固定相,分别采用2 mL/min及1.5 mL/min 的流动相流速、800 r/min的转速对独角莲中的有效成分皂苷进行分离,得到纯度98%的胡萝卜苷6 mg. 相似文献
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建立了高速逆流色谱(HSCCC)分离制备紫锥菊花色苷类化合物的方法,并对所获得的2个花色苷单体进行了体外抗氧化性实验。以新鲜紫锥菊花瓣为原料,含0.1%HCl的60%乙醇为溶剂避光冷浸提取,经乙酸乙酯萃取和D101大孔吸附树脂(100 mL,2 cm×30 cm)纯化后,得2.1 g紫锥菊花色苷提取物干粉样品。以水-正丁醇-甲基叔丁基甲醚-乙腈-三氟乙酸(6∶3∶2∶1∶0.001)为HSCCC分离溶剂系统,上相为固定相,下相为流动相,流速2.0 mL/min,进样量160 mg,通过一次分离得到2种花色苷单体化合物,经HPLC检测其纯度分别达95.1%(9.8 mg)、98.2%(14.3 mg),MS及NMR技术鉴定其结构分别为矢车菊素-3-O-β-D葡萄糖苷(化合物1)和矢车菊素-3-O-(6″-O-丙二酰-β-D葡萄糖苷)(化合物2)。以Vc为对照组,对所获得的2种花色苷单体化合物进行了1,1-二苯基-2苦肼基(DPPH.)体外抗氧化性能评价,结果显示2种花色苷对DPPH.的半清除率(EC50)均小于10 mg/L,小于对照样Vc,表明2种花色苷均具有较强的自由基清除作用,且化合物1的清除能力强于化合物2。 相似文献
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建立了薄层色谱图像分析定量-高速逆流色谱法从吴茱萸甲醇提取物中快速分离制备吴茱萸碱、吴茱萸次碱、吴茱萸卡品碱3个化合物的方法。采用数码相机对HSCCC溶剂系统上下相中的目标化合物进行TLC图像采集,使用积分软件OPSIA计算各溶剂系统对应的K值,筛选出最佳溶剂系统正己烷-乙酸乙酯-甲醇-水(3:2.5:3.5:2,V/V)。取上相为固定相,下相为流动相,检测波长为254 nm,在主机转速860 r/min、流动相流速1.5 mL/min的条件下,一次性从300 mg样品中分离制备得到经1H-NMR和13C-NMR确证的吴茱萸碱(15.3mg)、吴茱萸次碱(10.1 mg)、吴茱萸卡品碱(20.7 mg),纯度分别为93.6%,97.3%和95.1%(HPLC法)。 相似文献
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基于高速逆流色谱(HSCCC)技术从玛咖中分离制备出两种芥子油苷,苄基芥子油苷(glucotropaeolin, GTL)和甲氧基苄基芥子油苷(glucolimnanthin, GLI)。使用正交设计试验对分离条件进行优化,采用高分辨质谱对制备的组分进行鉴定,采用高效液相色谱法(HPLC)对组分进行定量分析。确定了两个组分GTL与GLI的HSCCC最佳分离条件:溶剂系统为正丁醇-乙腈-200 g/L硫酸铵溶液(1:0.5:2.4, v/v/v),上相为固定相,下相为流动相,流动相流速2 mL/min,主机转速900 r/min,从玛咖根粗提物中一次性分离得到157.72 mg/kg纯度为97.9%的苄基芥子油苷和31.93 mg/kg的甲氧基苄基芥子油苷,固定相保留率达57.6%。该方法成本低,简便易行,样品损失量小,可大量循环进样制备。 相似文献
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Uroš Grošelj Mojca Žorž Amalija Golobič Branko Stanovnik Jurij Svete 《Tetrahedron》2013,69(52):11092-11108
A new and simple synthesis of novel N-protected methyl 5-substituted-4-hydroxypyrrole-3-carboxylates, which exist in equilibrium with their 4-oxo tautomers, has been developed in two steps starting from N-protected α-amino acids. The key intermediates are enaminones, which can also be isolated, characterized, and used for the construction of other functionalized heterocycles, before they spontaneously decompose to pyrrole products. 4-Hydroxypyrroles are prone to partial aerial oxidation but can be efficiently alkylated or reduced to stable polysubstituted pyrrolidine derivatives. 相似文献
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The chemoselectivity in the intramolecular CH insertion of various diazosulfonamides has been experimentally studied. The results reveal that the aliphatic 1,4-, 1,5-, or 1,6-C(sp3)?H insertions of diazosulfonamides are not accessible, while the aromatic 1,5-C(sp2)?H insertion can be realized specifically by adjusting the diazo-adjacent group. In addition, the general chemoselectivities in the intramolecular CH insertions of diazosulfonyl compounds are summarized. Generally, diazosulfones undergo both aromatic 1,5-C(sp2)?H and aliphatic 1,5- and 1,6-C(sp3)?H insertions, while diazosulfonates undergo aliphatic 1,5- and 1,6-C(sp3)?H insertions. However, diazosulfonamides only undergo aromatic 1,5-C(sp2)?H insertion. 相似文献
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N-Heterocyclic carbene-palladacyclic complexes 3 were successfully achieved in a one-pot procedure under mild conditions. The structure of 3a was unambiguously confirmed by X-ray single crystal diffraction and it was an active catalyst in the Buchwald-Hartwig amination and α-arylation of ketones even at very low catalyst loadings (0.01?mol%). 相似文献
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Shashikant U. Dighe Surya K. Samanta Shivalinga Kolle Sanjay Batra 《Tetrahedron》2017,73(17):2455-2467
An efficient iodine-mediated oxidative Pictet-Spengler reaction in dimethyl sulphoxide (DMSO) using terminal alkynes as the 2-oxoaldehyde surrogate for the synthesis of aryl (9H-pyrido[3,4-b]indol-1-yl)methanones is described. The scope of the protocol includes the total synthesis of Fascaplysin, Eudistomins Y1 and Y2. The methodology is extended for preparing pyrrolo[1,2-a]-quinoxaline and indolo[1,5-a]quinoxaline derivatives. The utility of 1-aroyl-β-carbolines was demonstrated by performing palladium-catalyzed β-carboline directed ortho-C(sp2)-H functionalization of the phenyl ring with thiomethyl (SMe) group using DMSO as source and for accessing 4-aryl-canthin-6-ones. 相似文献
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In this Letter, we described a facile method for constructing fused bicyclic 1-arylpyrazol-5-one ring system. We employed various methylene-containing carboxylic acids as the substrates and proved that the pyrazolone ring closure requires activated methylene group in intermediate II. Accordingly, a series of structurally diversified, fused bicyclic 1-arylpyrazol-5-ones was prepared in moderate to high yields using the requisite substrates. 相似文献
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Synthesis of substituted pyrrolo[1,2-a]pyrazines and pyrazino[1,2-a]indoles from the Morita-Baylis-Hillman derivatives of acrylates via saponification followed by Curtius reaction is described. 相似文献
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用正丁胺作为碳源,采用射频辉光放电制备碳膜,选用激光染料R6G和聚乙二醇混合液作为蒸气源,采用单源热蒸发,在蒸发室与染料同时沉积得到混合膜,用拉曼光谱和红外光谱分析了碳膜的结构和键合方式,分析表明:碳膜中存在胺基团和氢原子.混合膜的荧光谱测量结果表明,认为正丁胺对染料荧光谱的影响是因为胺基和氢原子的存在. 相似文献
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Jona Mirnik Eva Pušavec Kirar Sebastijan Ričko Uroš Grošelj Amalija Golobič Franc Požgan Bogdan Štefane Jurij Svete 《Tetrahedron》2017,73(24):3329-3337
A series of 20 CuAIAC reactions between eight 4-acylamino substituted pyrazolidine-3-one-1-azomethine imines and four terminal ynones were performed using Cu0 as catalyst. The corresponding fluorescent cycloadducts were obtained in very high yields upon simple workup. Thus, Cu-metal turned out to be a better catalyst than CuI in terms of yield and ease of isolation. Availability of azomethine imines, mild reaction conditions, and simple workup enable a “click” access to libraries of densely substituted 2,3-dihydro-1H,5H-pyrazolo[1,2-a]pyrazol-1-ones. Reactivity of differently substituted dipoles was evaluated experimentally and by quantum chemical methods (DFT). 相似文献
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George E. Magoulas Thomas Garnelis Constantinos M. Athanassopoulos Dionissios Papaioannou George Mattheolabakis Konstantinos Avgoustakis Dimitra Hadjipavlou-Litina 《Tetrahedron》2012,68(35):7041-7049
(E)-4-(Fullerenopyrrolidin-1-yl)-3-methylbut-2-enoic acid and its corresponding succinimidyl ester, readily obtained through Prato-type modification of C60, were used for the selective N-acylation of polyamines. The thus obtained conjugates were evaluated for their antioxidative and anti-inflammatory activity and their cytotoxicity was determined. Members of this family of compounds showed interesting anti-lipid peroxidation, anti-lipoxygenase and anti-inflammatory activity and comparable cytocompatibility to spermidine. 相似文献