黑豆皮花色苷的中压液相色谱制备及结构鉴定

以黑豆皮为实验材料,用乙醇浸提法对黑豆皮中的花色苷进行提取,用大孔吸附树脂对花色苷进行纯化,经冷冻干燥得到黑豆皮花色苷粗品。利用中压制备色谱对花色苷组分进行分离,通过质谱分析鉴定经中压制备色谱分离后的花色苷组分。结果表明:黑豆皮花色苷粗品中的总花色苷含量为26.9%,经中压制备色谱对花色苷粗品进行分离后的2峰中矢车菊素-3-葡萄糖苷纯度达到91.46%。黑豆皮中的主要花色苷为天竺葵素-3-O-芸香糖苷、芍药色素-3-O-葡萄糖苷、矢车菊素-3-O-葡萄糖苷和锦葵素-3-葡萄糖苷-4-乙醛。     

凝胶柱色谱法分离纯化藜蒿中的黄酮苷类化合物

目的：研究鄱阳湖野生藜蒿中黄酮苷类化合物的分离纯化和结构鉴定。方法：采用超声辅助溶剂提取法提取藜蒿中的化学成分;采用聚酰胺柱层析法分离藜蒿中的黄酮苷元和黄酮苷类化合物;采用凝胶柱色谱法分离纯化藜蒿中的黄酮苷类单体化合物,根据化合物的理化性质和波谱特征鉴定化合物的化学结构。结果：藜蒿提取物中的黄酮苷元和黄酮苷类化合物得到较好的分离,同时分离并坚定了两个黄酮苷类的单体化合物——柯依利素-7-O- β-D- 葡萄糖苷和槲皮素-3-O- β-D- 木糖苷。结论：采用微波辅助溶剂提取结合聚酰胺柱层析可以充分提取并有效分离藜蒿提取物中的黄酮苷元和黄酮苷类化合物,采用凝胶柱色谱分离法可以分离制备藜蒿黄酮苷类单体化合物。     

荔枝核降糖活性部位化学成分的研究(Ⅰ)

目的:研究荔枝核降糖部位的化学成分。方法:采用α-葡萄糖苷酶活性测定法对荔枝核各提取部位进行活性筛选。通过多种色谱等手段对活性部位进行分离纯化,波谱分析及文献对照鉴定化合物的结构。结果:从荔枝核降糖的活性部位中分离并鉴定了8个化合物,分别为乔松素-7-O-β-D-葡萄糖苷(1),金粉蕨素(2),槲皮素(3),原儿茶醛(4),原儿茶酸(5),D-1-O-甲基-肌-肌醇(6),胡萝卜苷(7),β-谷甾醇(8)。结论:化合物1、3为首次从该植物中分离得到。     

夏桑菊复方化学成分的研究

目的研究夏桑菊复方的化学成分。方法通过各种柱色谱分离成分,依据理化性质和波谱方法鉴定化合物结构。结果从夏桑菊复方中分离鉴定了13个化合物,分别为:β-谷甾醇(1),β-胡萝卜苷(2),三十二烷酸(3),二十四烷醇(4),熊果酸(5),β-香树脂醇(6),山奈酚(7),槲皮素(8),木犀草素(9),紫云英苷(10),4′-甲氧基-芹菜素-7-O-β-D-吡喃葡萄糖苷(11),槲皮素-3-O-β-葡萄糖苷(12),蒙花苷(13)。结论化合物1-13为首次从该复方中分离得到。     

贵州烤烟糖苷类化学成分抗氧化活性及分离鉴定

为深入研究烟草糖苷类化学成分及其抗氧化活性,以贵州烤烟为材料,首先用有机溶剂甲醇回流提取和大孔树脂吸附法获得糖苷类化学成分粗提物,对糖苷粗提物不同溶剂萃取物的清除DPPH自由基活性进行研究,再应用反相色谱、凝胶色谱、半制备液相色谱及薄层层析等技术,对清除自由基活性最好的组分进行进一步分离纯化。结果表明,糖苷粗提物不同溶剂萃取物均表现一定的清除DPPH自由基活性,其中乙酸乙酯部分活性最好。从乙酸乙酯部分分离获得了多个糖苷类单体,并利用核磁共振仪对其中4个单体结构进行了鉴定,分别为7,8-二氢-3-氧代-α-紫罗兰醇-β-D-吡喃葡萄糖苷(化合物1),3-氧代-α-紫罗兰醇-β-D-吡喃葡萄糖苷(化合物2),异嗪皮啶6-O-β-D-吡喃葡萄糖苷(化合物3),东莨菪苷(化合物4)。     

茯砖茶中黄酮类化合物的分离与鉴定

本文采用高速逆流色谱与制备液相联用技术分离茯砖茶中黄酮类化合物。高速逆流色谱以正丁醇/乙酸乙酯/乙腈/0.5%乙酸水=12:2:3:15(V/V)为溶剂体系,将茯砖茶提取物分成7个流分,各流分经制备液相分离,获到19个化合物,利用波谱方法鉴定了15个化合物,均为黄酮类化合物:分别为芹菜素-6,8-二-C-β-D-葡萄糖(1),芹菜素-6-C-α-L-阿拉伯糖-8-C-β-D-葡萄糖(2),芹菜素-7-O-β-D-半乳糖-8-C-β-D-葡萄糖苷(3),槲皮素-3-O-葡萄糖-(1-3)-鼠李糖-(1-6)-葡萄糖(4),山奈酚-3-O-β-D-葡萄糖-(1-3)-α-L-鼠李糖-(1-6)-β-D-葡萄糖苷(5),芹菜素-7-O-α-L-鼠李糖-8-C-β-D-半乳糖(6),芦丁(7),山奈酚-3-O-α-L-鼠李糖(1-6)-β-D-葡萄糖苷(8),Camelliquercetiside A(10),杨梅素3-O-β-D-葡萄糖苷(12),异牡荆苷(13),牡荆苷(15),槲皮素3-O-β-D-葡萄糖苷(16),Camelliquercetiside C(17),山奈酚-3-O-β-D-半乳糖苷(18),其中化合物3和6为新黄酮碳苷化合物,化合物1为茶叶中首次发现。     

紫斑牡丹籽饼粕单萜苷类成分的分离鉴定

目的:研究紫斑牡丹榨油后的籽饼粕单萜苷类化学成分的分离鉴定,探索油用牡丹籽油制备过程中的副产物——牡丹籽饼粕的研究开发价值。方法:采用硅胶、凝胶柱色谱以及半制备高效液相色谱等技术进行分离纯化,综合运用波谱学方法鉴定化合物的结构。结果:从油用牡丹籽饼粕中共分离的8个单萜苷类化合物,分别鉴定为β-gentiobiosyl-paeoniflorin(1)、白芍苷(2)、氧化白芍苷(3)、牡丹酮-1-O-β-D-吡喃葡萄糖苷(4)、白芍苷R1(5)、paeonifanin(6)、8-O-去苯甲酰白芍苷(7)、牡丹皮苷F(8)。结论:上述8个化合物均为首次从紫斑牡丹榨油后的牡丹籽饼粕中分离得到。结果表明油用牡丹籽饼粕中含有大量的单萜苷类化合物,具有重要的研究开发价值。     

七叶一枝花的化学成分研究

目的研究七叶一枝花Paris polyphylla Smith var.chinensis(Franch.)Hara的化学成分。方法溶剂提取后,利用正相硅胶色谱,反向制备色谱,ODS柱色谱等手段对该植物的乙酸乙酯和正丁醇部位提取物进行分离与纯化,并通过核磁共振碳谱(~(13)C NMR),核磁共振氢谱(~~1H NMR)和电子轰击质谱(EI-MS)等波谱技术进行结构鉴定。结果从乙酸乙酯层和正丁醇层分离得到10个化合物,经分离鉴定为β-谷甾醇(Ⅰ),槲皮素(Ⅱ),胡萝卜苷(Ⅲ),豆甾醇(Ⅳ),偏诺皂苷元-3-O-α-L-呋喃阿拉伯糖基-(1→4)-α-L-吡喃鼠李糖基-(1→2)-β-D-葡萄糖苷(Ⅴ),熊果酸(Ⅵ),薯蓣皂苷元-3-O-α-L-呋喃阿拉伯糖基-(1→4)-α-L-吡喃鼠李糖基-(1→2)-β-D-吡喃葡糖苷(Ⅶ),葡萄糖(Ⅷ),薯蓣皂苷元-3-O-α-L-吡喃鼠李糖基-(1→4)-α-L-吡喃鼠李糖基-(1→2)-β-D-葡萄糖苷(Ⅸ),山奈酚(Ⅹ)。结论化合物Ⅱ,Ⅹ为种首发,化合物Ⅵ,Ⅷ为属首发。     

常春油麻藤花黄酮类化合物结构鉴定及抗氧化活性分析

目的:阐明常春油麻藤(Mucuna sempervirens)花中的黄酮类化合物及其抗氧化活性。方法:利用高速逆流色谱、制备型液相色谱等技术进行分离纯化,根据化合物的理化性质和波谱数据进行结构鉴定,并采用DPPH法测定其抗氧化活性。结果:分离得到8个化合物单体,鉴定为矢车菊3-O-6'-O-α-鼠李糖-β-D-葡萄糖苷(cyanidin3-O-6'-O-α-rhamnopyranosyl-β-D-glucopyranoside,I)、矢车菊3-O-β-D-葡萄糖苷(cyanidin 3-O-β-D-glucopyranoside,II)、槲皮素-3-O-β-D-葡萄糖苷(quercetin-3-O-β-D-glucopyranoside,III)、二氢槲皮素(dihydroquercetin,IV)、山奈酚(kaempferol,V)、异夏佛塔苷(6-C-β-L-arabinopyranosyl-8-C-β-D-glucopyranosyl apigeni,VI)、山奈酚-33-O-α-L-鼠李糖基-(1-6)-β-D-半乳糖苷(kaempferol-3-O-α-L-rhamnopyranosyl-(1-...     

毛泡桐果化学成分研究

目的研究毛泡桐果实的化学成分。方法应用柱色谱方法分离和纯化,通过理化常数和波谱分析鉴定化合物的结构。结果从毛泡桐果中分离出11个化合物,其结构分别鉴定为:β-谷甾醇(Ⅰ),泡桐素(Ⅱ),熊果酸(Ⅲ),胡萝卜苷(Ⅳ),芹菜素(Ⅴ),香草酸(Ⅵ),异香草酸(Ⅶ),对羟基苯甲酸(Ⅷ),5,7,4′-三羟基-3′-甲氧基黄酮(Ⅸ),3′-甲氧基木犀草素-7-O-β-D葡萄糖苷(Ⅹ),diplacone(Ⅺ)。结论化合物Ⅵ、Ⅶ为首次从该属中分得,化合物Ⅱ、Ⅸ、Ⅹ为首次从毛泡桐果中分得。     

张家界桑植浓香型烤烟烟叶分切研究

采用TG-DTA、GC/MS等技术对湖南桑植浓香型烤烟烟叶分切后的叶尖、中间及叶基部位进行热反应分析以及常规化学成分、挥发性成分检测,并以烟叶常规化学成分和挥发性成分为指标进行分切段及全叶烟叶聚类分析。结果表明:①烟叶分切后,各段烟叶常规化学成分含量、挥发性成分相对百分含量、热失重比存在明显差异。叶尖部分烟叶的烟碱含量最高,叶尖和中间部分烟叶的还原糖和总糖含量较高,叶基部分烟叶的钾、氯和总氮含量较高。叶尖部分烟叶的茄哪士酮和棕榈酸含量较高,中间部分烟叶的苯甲醇、香叶基丙酮和肉豆蔻酸含量较高,叶基部分烟叶的新植二烯、3-呋喃甲醛、巨豆三烯酮和亚麻酸甲酯含量较高。中间部分烟叶热失重率最高,叶基部分最低。②不同的分切段烟叶可聚类到不同的类别,烟叶分切后可以形成不同的配方模块,拓宽烟叶原料使用范围,提高卷烟原料的保障能力。     

Using Both Chemical and Biological Fingerprints for the Quality Study of Estrogenic Licorice (Glycyrrhiza uralensis)

ABSTRACT: The quality of phytoestrogenic licorice was studied by using both chemical and biological fingerprints. A recombinant yeast strain that consists of an estrogen responsive element linked with a reporter gene ( ADE2 ) and a transformed human estrogen receptor–containing plasmid was used for screening and evaluation of estrogenic activity in licorice. Several estrogen-like components in licorice were screened, and licoisoflavone B and formononetin were identified. Licorice extracted with 70% ethanol showed 5 different patterns of chemical fingerprints (LR-A, LR-E, LR-F, LR-H, LR-K), as identified by chromatographic analysis. Among these, LR-E exhibited the strongest estrogenic activity, whereas LR-A, LR-F, and LR-H were in the middle, and LR-K had the weakest activity.     

罗汉果饮料的生产工艺研究

初步介绍罗汉果的外貌、生理习性和罗汉果化学成分、药理作用。详细介绍了罗汉果原液的提取分离技术以及饮料的制作工艺。饮料以罗汉果浸提液为主要原料,添加适量的调味剂调制而成。3000mL的饮料中原液:180mL;木糖醇:120g;柠檬酸:0.4g;干草浸提液:20mL。这种饮料低脂,不含蔗糖,口感清爽,适合糖尿病人、肥胖病人饮用,具有一定的市场发展前景。     

Sweetened Mango Purees Preserved by Canning and Freezing

Mango fruit (Mangifera indica L., Kent variety) at canning ripeness was processed as sweetened puree of 42–43° Brix soluble solids by canning and freezing. Sucrose and high fructose corn syrups in various combinations were used as sweeteners. Processed purees, diluted with three parts of water, produced mango nectars of 13% soluble solids for evaluation of chemical and sensory quality. The frozen mango purees contained slightly more ascorbic acid than the canned products. Sucrose and high fructose corn syrups may be used interchangeably as sweeteners. Panel members were not able to distinguish differences in preference for nectars even though some difference in sugar components among them were detected by high performance liquid chromatography.     

超临界CO_2萃取与浸渍法制备白刺果油及其化学成分的分析与比较

为了促进白刺属植物在医药、食品、化工等领域中的应用,文中采用超临界CO2流体萃取法和溶剂浸渍法提取西伯利亚白刺果油,并用气相色谱-质谱联用技术(GC-MS)对其化学成分进行了分析,从超临界CO2萃取、浸渍法提取出的白刺果油中分别鉴定出26种成分。主要化学成分是亚油酸、油酸、γ-生育酚、VE(α-生育酚)、菜油甾醇、γ-谷甾醇、二十八碳烷、二十七碳烷等。     

Antioxidant and anti‐inflammatory activities of water distillate and its dichloromethane extract from licorice root (Glycyrrhiza uralensis) and chemical composition of dichloromethane extract

BACKGROUND: Licorice root is one of the most widely used medicinal herbs and its medicinal properties, such as antibacterial, anti‐ulcer, anti‐tumorigenic and anti‐atherosclerotic activities, have been widely reported. However, there are only a few reports on basic chemical and biological studies of the water distilled components of licorice root. RESULTS: Chinese licorice root was water distilled and the distillate was subsequently extracted with dichloromethane. Residual aqueous solution from the extraction was fractionated using column chromatography. A total of 127 chemicals were identified in the dichloromethane extract, which inhibited hexanal oxidation by over 90% for 45 days at the level of 50 µg mL^?1. A fraction eluted from the residual aqueous solution with acetone exhibited potent antioxidant activities both in a thiobarbituric acid assay and in a malonaldehyde/gas chromatography assay. The acetone fraction also exhibited strong anti‐inflammatory activity (77.9% inhibition at the level of 62 µg mL^?1) in a lipoxygenenase inhibitor screening anti‐inflammatory assay. CONCLUSION: This study demonstrated the antioxidant and anti‐inflammatory activities of the water distillate obtained from Chinese licorice root. Some volatile chemicals among the many components identified in the water distillate exhibited antioxidant activity, suggesting that many medicinal compounds escape with water vapor into the ambient air during the preparation of herbal medicine. Copyright © 2008 Society of Chemical Industry     

Membrane-based separation scheme for processing sweeteners from stevia leaves

In existing processes, extraction and refining of glycoside based sweeteners from stevia leaves involves many process steps including extraction by organic solvents. The purpose of the present study was to develop a process of extraction and refining of sweeteners with reduced number of unit operations and minimization and/or elimination of chemical usage including organic solvents. It was found that water was very effective for extracting glycosides at selected pH and temperatures. It was also shown that a multi-stage membrane process was successfully able to concentrate the glycoside sweeteners. Based on the preliminary results, it appears that bitter-tasting components were washed out from the sweetener concentrate in the nanofiltration process. This work also has demonstrated that a membrane-based separation process for refining glycoside-based sweeteners could be viable and needs to be investigated further.     

旋覆花挥发油成分的GC-MS分析

采用水蒸气蒸馏法提取旋覆花全草挥发油,出油率为0.32%。采用GC-MS联用技术对挥发油成分进行分离鉴定,面积归一化法确定各成分的相对含量,从其中鉴定出34个化学成分,鉴定成分占总峰面积的99.85%。旋覆花挥发油的主要化学成分分别为植酮(21.75%)、长叶烯(9.71%)、棕榈酸(7.98%)、邻苯二甲酸二丁酯(7.40%)、肉豆蔻酸(7.38%)、2,6-二甲基-4-甲氧基甲基苯酚(7.04%)、2-(对-茴香基)-4-甲基己烯(5.26%)、石竹素(5.03%)、邻苯二甲酸二异丁酯(4.75%)等。鉴定出的34种成分中脂肪类占45.5%,芳香类成分占26.74%,萜类占26.43%,其他类占1.18%。     

甘草酸和甘草次酸提取分离方法的研究进展

甘草是豆科多年生草本植物,甘草酸和甘草次酸等三萜类化合物是甘草的主要成分,为药食两用植物。本文综述了近10年甘草三萜类化合物中甘草酸和甘草次酸的提取及分离纯化方法,提取方法包括溶剂提取法、超声辅助提取法、微波辅助提取法和半仿生-酶提取法等,分离纯化方法包括重结晶法、大孔树脂法、膜分离法和固相萃取法等。针对甘草药材来源及甘草酸提取工艺考查指标混乱等问题进行了归纳总结,以期为甘草酸和甘草次酸提取分离的后续研究提供参考。     

Isolation and identification of main constituents in an enzymatically hydrolysed licorice extract sweetener

Licorice extract including glycyrrhizin as the major component is used as a safe sweetener in many countries. Enzymatically hydrolysed licorice extract (EHLE) is also used as a sweetener in Japan. In the present paper, the constituents of EHLE were investigated as a part of the studies for evaluating its quality and safety as a food additive. Three oleanane-type monoglycosides along with glycyrrhizin (1) eand 3-O-[beta-D-glucuronopyranosyl-(1-->2)-beta-D-glucuronopyranosyl]-18beta-liquiritic acid (2) were isolated from EHLE. The structures of the three compounds have been determined to be 3-O-beta-D-glucuronopyranosyl-24-hydroxy-18beta-glycyrrhetinic acid (3), 3-O-beta-D-glucur-onopyranosyl-18beta-glycyrrhetinic acid (4) and 3-O-beta-D-glucuronopyranosyl-18beta-liquiritic acid (5) based on MS and NMR. Compound 4 was the monoglycosylated derivactive of glycyrrhizin (1). Compounds 3 amd 5 are the monoglycosylated derivatives of the minor constituents in licorice extract. They were first isolated from EHLE, and compound 5 was a new compound.