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1.
采用高速逆流色谱结合制备液相色谱法从葡萄籽乙醇提取物中分离得到了8种多酚。高速逆流色谱以上相为固定相,下相为流动相,主机转速为900 r/min,流速为2 mL/min,分离温度为25℃,检测波长为280 nm,利用正向和反向洗脱相结合的模式,在正丁醇-乙酸乙酯-水(1∶14∶15,v/v/v)和正己烷-乙酸乙酯-水(1∶10∶10,v/v/v)溶剂系统下从葡萄籽提取物中分离得到了5种多酚。原花青素B1、原花青素B2、没食子酸、表儿茶素没食子酸酯和儿茶素的纯度分别为98.5%、97.2%、98.3%、98.9%和96.7%。利用制备液相色谱法对高速逆流色谱分离成分进一步分离纯化,获得了表儿茶素、表没食子儿茶素没食子酸酯和没食子儿茶素没食子酸酯,纯度分别99.2%、99.3%和99.2%。该方法单次制备量均达到毫克级,简便、快速、分离纯度高,适合于葡萄籽中多酚的分离制备。 相似文献
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氧化巴西木素是苏木的主要化学成分之一,具有广泛的药理活性且常作为染色剂应用于各行各业。采用传统柱色谱法进行分离,不仅会造成色谱柱材料的污染,也会造成活性成分的损失。故采用高效逆流色谱(HPCCC)对苏木中的活性化合物氧化巴西木素进行分离纯化。苏木乙醇提取物经乙酸乙酯萃取后直接进行高效逆流色谱分离。首先利用基于薄层色谱的常用溶剂体系估算法和摇瓶法结合高效逆流色谱分析模式进行溶剂体系筛选。结果表明,最佳溶剂体系为氯仿-甲醇-水(4∶3∶2, v/v/v)。高效逆流色谱以反相模式为洗脱模式,主机转速为1 600 r/min,流速为10 mL/min,分离温度为25℃,检测波长为285 nm,在氯仿-甲醇-水(4∶3∶2, v/v/v)溶剂体系下,从500 mg苏木乙酸乙酯萃取物中一次性分离制备得到15.2 mg纯度为95.6%的氧化巴西木素及一微量成分caesappanin C。采用高效逆流色谱分离制备氧化巴西木素,可避免苏木中的活性成分氧化巴西木素对色谱柱中的固体填充材料染色和难以洗脱等问题,并缩短分离纯化工作时间,提高工作效率。故可将高效逆流色谱应用到苏木中其他色素化合物或其他染料植物的... 相似文献
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眼镜蛇蛇油中甘油三酸酯的成分研究 总被引:1,自引:0,他引:1
用AgNO3-硅胶薄层板,氯仿+丙酮(20+1)为展开剂,将蛇油中甘油三酸酯分离为5个组分,并用同样的色谱固定相和石油醚-氯仿-丙酮溶剂系统进行制备性分离。用质谱法对甘油三酸酯进行分子一级水平的化学研究,确定了眼镜蛇蛇油中5个主要的甘油三酸酯成分的结构形式为:16∶0-18∶0-18∶0,16∶0-18∶0-18∶1,16∶0-18∶2-18∶1,18∶2-18∶2-18∶0,18∶2-18∶2-18∶1。 相似文献
4.
高速逆流色谱法分离制备乌药叶中的黄酮类成分 总被引:3,自引:0,他引:3
应用高速逆流色谱法分离制备了乌药叶中的黄酮类成分。以正己烷-乙酸乙酯-正丁醇-冰醋酸-水(体积比为2∶4∶2∶1.5∶6)为两相溶剂系统,在主机转速800 r/min、流速2.0 mL/min、检测波长280 nm条件下进行分离制备。所得流分经高效液相色谱法检测,并经电喷雾电离质谱、核磁共振氢谱、碳谱鉴定化合物的结构。结果表明,从乌药叶总黄酮粗提物中分离得到了5个化合物,分别为槲皮素-3-O-β-D-葡萄糖苷(1)、槲皮素-5-O-β-D-葡萄糖苷(2)、槲皮素-3-O-β-D-呋喃阿拉伯糖苷(3)、槲皮素-3-O-吡喃鼠李糖苷(4)、山奈酚-7-O-α-L-吡喃鼠李糖苷(5),其中化合物1,2,3和5 为首次从该植物中分离得到。该法具有简便、快速的优点。 相似文献
5.
微柱高效液相色谱法分离八角茴香挥发油成分 总被引:9,自引:1,他引:8
利用微柱高效液相色谱法(μ-HPLC)对八角茴香果实挥发油成分进行了分离,对固定相类型、流动相组成及流速等条件进行了优化。结果表明,选用氰基分析柱(250mm×0.32mmi.d.,5μm),正己烷-乙腈-二氯甲烷(80∶8∶12,体积比)为流动相,流速为2μL·min-1,八角茴香果实挥发油成分在微柱液相色谱上分离效果最好。在优化的实验条件下,对实际样品中反式-茴香醚、茴香醛等成分进行了定量。本实验为以后的μ-HPLC与毛细管气相色谱联用分析植物挥发油奠定了基础。 相似文献
6.
正交轴逆流色谱法分离标准蛋白质及实际样品 总被引:3,自引:1,他引:3
以m(质量分数为 12 .5 %的PEG80 0 0 )∶m(质量分数为 2 5 %的磷酸氢二钾 ) =1∶1或m(质量分数为 12 .5 %的PEG80 0 0 )∶m(质量分数为 30 %的磷酸氢二钾 ) =1∶1为溶剂系统 ,用下相作流动相 ,上相作固定相 ,操作时采用5 0 0r/min的转速和 6 0mL/h的流动相流速 ,考察了正交轴逆流色谱法对标准蛋白质及羊肚菌糖蛋白和枸杞糖肽的分离情况。将结果与高效液相色谱分离结果相比较 ,前者在分离度损失不大的基础上提高了进样量 ,证明了其用于制备的有效性 ,从而为分离制备天然生物大分子提供了一个新方法。 相似文献
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反相高效液相色谱法制备银杏叶中聚戊烯醇同系物单体 总被引:1,自引:0,他引:1
利用制备高效液相色谱法从银杏叶中分离制备了聚戊烯醇同系物单体。在HiQ sil C18柱上,以异丙醇-甲醇-正己烷-水(体积比为50∶25∶15∶4)为流动相,流速10 mL/min,采用等度洗脱方式,制备了8种化合物,经紫外光谱、红外光谱及质谱分析,确认它们分别为C70,C75,C80,C85,C90,C95,C100和C105聚戊烯醇,其中主要成分为C85及C90聚戊烯醇。高效液相色谱分析表明,制备的C75C105聚戊烯醇化合物的纯度均在96%(质量分数)以上。在该色谱条件下,各色谱峰达到了基线分离, 相似文献
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首次以二甲亚砜/正十二醇为二元致孔剂,苯乙烯为单体,二乙烯苯为交联剂,过氧化苯甲酰为引发剂,通过原位聚合反应制备了苯乙烯-二乙烯苯聚合物型毛细管整体柱。结果表明,苯乙烯∶二乙烯苯∶二甲亚砜∶正十二醇的体积比为18.7∶15.3∶13.2∶52.8,即二甲亚砜占致孔剂的比例为20%,交联度为45%,致孔剂含量为66%为最优配比。所合成的整体柱实现了反相色谱模式下对小分子苯系物与生物大分子蛋白的快速分离。其中蛋白分离实验的流速达到104μL·min-1,线速度约为12 mm·s-1,而常规色谱柱的线速度为1~2 mm·s-1。该整体柱的渗透性好,可用于物质的高速分离,若对其进行化学修饰,有望用于其它色谱分离模式。 相似文献
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An efficient method for bioassay-guided preparative isolation of antioxidants from the n-butanol extract of Astragalus altaicus Bunge was ingeniously developed by combination of silica gel column chromatography and high-speed counter-current chromatography. Under the bioassay-guidance of antioxidant activities, the antioxidants were gradually separated from the crude sample of Astragalus altaicus Bunge by silica gel column chromatography and high-speed counter-current chromatography. Silica gel column chromatography separation was performed with chloroform, chloroform-methanol (100:1~5:1, v/v) and chloroform-methanol-water (5:1:0.1~2:1:0.1, v/v/v). High-speed counter-current chromatography separation was performed with a two-phase solvent system composed of ethyl acetate-n-butanol-water (2:1:6, v/v/v), which was successfully selected by thin layer chromatography analysis, at a flow rate of 1.5 mL/min. As a result, isorhamnetin-3-gentiobioside (20.8 mg), rutin (82.0 mg), and narcissin (12.8 mg) were obtained for the first time from 200 mg of the crude sample, ABS-5 of Astragalus altaicus Bunge. The purities were all at over 95% by high-performance liquid chromatography analysis, and their structures were unambiguously identified by mass spectroscopy, (1) H, and (13) C nuclear magnetic resonance spectroscopy. Antioxidant activities of the three compounds were also assayed by in vitro ABTS [2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulphonic acid) diamonium salt] radical cation scavenging activity. Among them, rutin possessed the highest antioxidant capacity with SC(50) value of 22.15 μg/mL. 相似文献
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Isolation of the lignan secoisolariciresinol diglucoside from flaxseed (Linum usitatissimum L.) by high-speed counter-current chromatography 总被引:1,自引:0,他引:1
High-speed counter-current chromatography was successfully used for the isolation and purification of secoisolariciresinol diglucoside, a bioactive lignan from flaxseed (Linum usitatissimum L.). The solvent system consisted of tert.-butylmethyl ether-n-butanol-acetonitrile-water (1:3:1:5). The purity and identity of the isolated compound was checked by high-performance liquid chromatography analysis in combination with mass spectrometry and NMR measurements. 相似文献
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《Journal of separation science》2017,40(6):1273-1282
10‐Deacetylbaccatin III, an important semisynthetic precursor of paclitaxel and docetaxel, can be extracted from Taxus wallichiana Zucc. A process for the isolation and purification of 10‐deacetylbaccatin III ( 1 ), baccatin III ( 2 ), and 7β‐xylosyl‐10‐deacetyltaxol ( 3 ) from the leaves and branches of Taxus wallichiana Zucc. via macroporous resin column chromatography combined with high‐speed countercurrent chromatography or reversed‐phase flash chromatography was developed in this study. After fractionation by macroporous resin column chromatography, 80% methanol fraction was selected based on high‐performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis. A solvent system composed of n‐hexane, ethyl acetate, methanol, and water (1.6:2.5:1.6:2.5, v/v/v/v) was used for the high‐speed countercurrent chromatography separation at a flow rate of 2.5 mL/min. The reversed‐phase flash chromatography separation was performed using methanol/water as the mobile phase at a flow rate of 3 mL/min. The high‐speed countercurrent chromatography separation produced compounds 1 (10.2 mg, 94.4%), 2 (2.1 mg, 98.0%), and 3 (4.6 mg, 98.8%) from 100 mg of sample within 110 min, while the reversed‐phase flash chromatography separation purified compounds 1 (9.8 mg, 95.6%) and 3 (4.9 mg, 97.9%) from 100 mg of sample within 120 min. 相似文献
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Separations of flavonoids and alkaloids in medicinal herbs by high-speed counter-current chromatography 总被引:1,自引:0,他引:1
Counter-current chromatography is a new liquid-liquid partition chromatography without using solid support. Recently, the technique has been remarkably improved in both partition efficiency and separation time. In this paper the capability of this high-speed counter-current chromatography was demonstrated on separation of two sets of samples obtained from medicinal herbs: a synthetic mixture of 3'-hydroxygenkwanin, luteolin and apigenin was separated on a two-phase solvent system composed of chloroform-methanol-water (4:3:2, v/v/v) and a crude ethanol extract from Anisodus tangulicus (Maxin) Pasch on chloroform-0.07 M sodium phosphate (pH 6.4) (1:1, v/v). In the light of chromatograms obtained from these samples, advantages of high-speed counter-current chromatography over other chromatographic methods were discussed in terms of partition efficiency, peak resolution, separation time, sample loading capacity, etc. 相似文献
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In this paper, the combined techniques of macroporous resin column chromatography and high speed counter-current chromatography were applied for preparative separation of flavonoid triglycosides from the leaves of Actinidia valvata Dunn, a famous Chinese medicinal herb. Twelve kinds of macroporous resins were investigated by adsorption and desorption tests. HPD-300 resin showed the maximum effectiveness and thus was selected for the first cleaning-up, in which 20% ethanol was used to remove the undesired constituents and 60% ethanol to elute the targets. The crude extract was then purified by high speed counter-current chromatography with the solvent system composed of ethyl acetate-n-butanol-water (2:1:3 and 4:1:5, v/v). Three flavonoid triglycosides, namely, kaempferol 3-O-α-L-rhamnopyranosyl-(1→3)-α-L-rhamnopyranosyl-(1→6)-β-D-galactopyranoside, kaempferol 3-O-α-L-rhamnopyranosyl-(1→3)-(4-O-acetyl-α-L-rhamnopyranosyl)-(1→6)-β-D-galactopyranoside and kaempferol 3-O-α-L-rhamnopyranosyl-(1→3)-(2,4-di-O-acetyl-α-L-rhamnopyranosyl)-(1→6)-β-D-galactopyranoside, were obtained. The purities of the separated compounds were all over 95% as determined by HPLC area normalization method. Their chemical structures were confirmed by UV, MS, NMR, and the standards. 相似文献
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Xue Yang Nana Wang Cheng Shen Hongmei Li Jingyang Zhao Tao Chen Yulin Li 《Journal of separation science》2019,42(3):684-690
The separation of minor compounds, especially those with similar polarities from a complex sample, remains challenging. In the proposed study, an effective method based on medium‐pressure liquid chromatography and recycling high‐speed counter‐current chromatography was developed for the enrichment and separation of three minor components from Dracocephalum tanguticum. The crude extract was directly introduced to medium‐pressure liquid chromatography for the enrichment of the three minor components. Based on high‐performance liquid chromatography analysis, the total content of these three compounds increased from 0.48% in the crude extract to 85.3% in the medium‐pressure liquid chromatography fraction. In addition, high‐speed counter‐current chromatography was employed to separate the enriched compounds using the solvent system hexane/ethyl acetate/methanol/water (1.18:8.82:1.18:8.82, v/v/v/v). As a result, compound 3 and a mixture of compounds 1 and 2 were obtained. In order to improve the resolution of compounds 1 and 2 while saving separation time, a recycling and heart‐cut mode was used. Finally, compounds 1 and 2 were obtained after five cycles. These compounds were identified as 3‐phenylethyl β‐d ‐glucopyranoside ( 1 ), tazettoside E ( 2 ), and cirsiliol‐4′‐glucoside ( 3 ). Compounds 1 and 2 were primarily separated from D. tanguticum. Moreover, the developed method provided a reference for the separation of minor components from the complex sample. 相似文献
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K.G. Blass 《Microchemical Journal》1984,30(2):147-153
The present study has confirmed the formation of picramic acid and methylguanidine during the heated Jaffe' reaction. Picramic acid was isolated on thin-layer chromatography from 0.5:1 and 1:1 heated creatinine:picric acid molar ratio test solutions, but not for similarly performed 3:1 test solutions. A Dowex column was employed to isolate methylguanidine from 0.5:1 and 3:1 molar ratio test solutions. Methylguanidine was similarly isolated from a heated alkaline creatinine solution. 相似文献
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Preparative separation of methyl gallate in leaves extract of Acer truncatum Bunge was conducted using high-speed counter-current chromatography (HSCCC) with a solvent system composed of ethyl acetate-ethanol-water at volume ratios of 5:1:5 (v/v/v). In a single operation, 57.5 mg of methyl gallate was obtained from 120 mg of the extract. HPLC analyses of the counter-current chromatography (CCC) fraction revealed that the methyl gallate was having over 97% purity. Its structure was identified by 1H NMR and 13C NMR. 相似文献
20.
Isolation of quercetin-3-O-L-rhamnoside from Acer truncatum Bunge by high-speed counter-current chromatography 总被引:2,自引:0,他引:2
Preparative high-speed counter-current chromatography (HSCCC) was successfully used for isolation and purification of quercetin-3-O-L-rhamnoside from the ethyl acetate extract of the leaves of Acer truncatum Bunge using a two-phase-system composed of ethyl acetate-ethanol-water at a volume ratio of 5:1:5 (v/v/v). In a single operation, 41.9mg of quercetin-3-O-L-rhamnoside was obtained from 366mg of the crude extract. High-performance liquid chromatography (HPLC) analyses of the CCC fraction revealed that the purity of quercetin-3-O-L-rhamnoside was over 96%. Its structure was identified by MS, 1H NMR and 13C NMR. Quercetin-3-O-L-rhamnoside was obtained from this plant for the first time. 相似文献