中药广藿香非挥发性化学成分的研究

目的:研究广藿香非挥发性部位的化学成分.方法:采用多种色谱技术分离纯化化合物,根据化合物的理化性质和波谱数据鉴定其结构.结果:从中药广藿香全草95%乙醇提取物的醋酸乙酯萃取部分分离得到9个化合物,分别鉴定为:表木栓醇(1),5-羟甲基糠醛(2),1,4-丁二酸(3),β-谷甾醇(4),胡萝卜苷(5),1,2-O-[2S-(3,4-二羟基苯基).1,2.乙烷二基]-3-D-a-L-鼠李毗喃糖基-4-O-咖啡酰基-β-D-葡萄毗喃糖苷(6)、1,2-O-[2S-(3,4-二羟基苯基)-1,2-乙烷二基]-3-D-a-L-鼠李毗喃糖基-4-O-阿魏酰基-β-D-葡萄毗喃糖苷(7)、1,2-O-[2S-(3,4-二羟基苯基)-1,2-乙烷二基]-3-O--a-L-鼠李毗喃糖基-6-O-咖啡酰基-β-D-葡萄毗喃糖苷(8)和芹菜素-7-O-β-D-(6"-对位香豆酰基)-葡萄糖苷(9).结论:化合物2,3,6～8均为首次从该属植物中分离得到.     

广藿香非挥发性化学成分的研究

目的:研究广藿香Pogostemon cablin的非挥发性化学成分。方法:采用硅胶、Sephadex LH-20等柱色谱方法进行分离纯化,并根据化合物的理化性质和波谱数据鉴定其结构。结果:从广藿香醇提物中分离得到12个化合物,分别鉴定为田蓟苷(1),香叶木素-7-O-β-D-吡喃葡萄糖苷(2),1,2-O-[2S-(3,4-二羟基苯基)-1,2-乙烷二基]-3-O-α-L-鼠李吡喃糖基-4-O-阿魏酰基-β-D-吡喃葡萄糖苷(3),尿嘧啶(4),大豆脑苷Ⅰ和Ⅱ(5),藿香苷(6),7-O-(3″,6″-二-反式-对-香豆酰基)-β-D-半乳糖-芹菜素苷(7),5-羟基-3,3′,4′,7-四甲氧基黄酮(8),4′,5-二羟基-3,3′,7-三甲氧基黄酮(9),金合欢素(10),1,2-O-[2S-(3,4-二羟基苯基)-1,2-乙烷二基]-3-O-α-L-鼠李吡喃糖基-4-O-咖啡酰基-β-D-吡喃葡萄糖苷(11),1,2-O-[2S-(3,4-二羟基苯基)-1,2-乙烷二基]-3-O-α-L-鼠李吡喃糖基-6-O-咖啡酰基-β-D-吡喃葡萄糖苷(12)。结论:化合物1,2,4~7,10为首次从该属植物中分离得到。     

龙须藤化学成分及其抗类风湿性关节炎活性研究

目的:研究龙须藤的化学成分及其对滑膜细胞的抑制作用。方法:运用硅胶柱层析、Sephadex LH-20凝胶柱色谱等方法,对龙须藤乙酸乙酯部位化学成分进行分离纯化,利用现代波谱学技术鉴定化合物结构,采用MTT法对分离得到的单体化合物进行体外抑制滑膜细胞增殖的活性筛选。结果:从龙须藤乙酸乙酯部位分离得到9个化合物,分别鉴定为:豆甾醇-4-烯-3-酮(1)、β-谷甾醇棕榈酸酯(2)、1-(2,4-二羟基苯基)-3-(3,4-二羟基苯基)-3-羟丙基-1-酮(3)、7-羟基香豆素(4)、没食子酸(5)、松柏醛(6)、1-(3,4-二甲氧基苯基)-1-丙醇(7)、丁香酸(8)、没食子酸乙酯(9)。结论:其中,化合物1～4、6、7、9为首次从龙须藤中分离得到,化合物1、3、6、7、9为首次从该属植物中分离得到。MTT法结果显示化合物1～9均对滑膜细胞具有一定的抑制作用,其中化合物5抑制作用最强。     

粉萆薢脂溶性化学成分研究

目的研究粉萆薢(粉背薯蓣Dioscorea hypoglauca干燥根茎)中的脂溶性化学成分。方法采用色谱法分离纯化化合物,理化性质和波谱数据鉴定化合物结构。结果从粉萆薢脂溶性部分中分离鉴定了13个化合物,包括3个二芳基庚烷类和一些其他类化合物,分别鉴定为7-(4-羟基-3-甲氧基苯基)-1-(4-羟基苯基)-4,6-庚烷-3-酮(1)、1,7-双-(4-羟基苯基)-1,4,6-庚三烯-3-酮(2)、1,7-双-(4-羟基苯基)-4,6-庚二烯-3-酮(3)、大黄素(4)、7-羟基-2,6-二甲氧基-1,4-菲醌(5)、薯蓣皂苷元(6)、鲁可斯皂苷元(7)、山柰酚(8)、(3S)-6,8-二羟基-3-苯基-3,4-二氢异香豆素(9)、5-羟甲基糠醛(10)、β-谷甾醇(11)、豆甾醇(12)、二十六烷酸(13)。结论化合物4、5、7、8、12、13为首次从粉萆薢中分离得到,化合物1、10为首次从薯蓣属植物中分离得到。     

牡荆子的化学成分

目的:研究牡荆子的化学成分。方法:采用反复硅胶柱色谱、ODS、制备高效液相色谱法及重结晶等方法对牡荆子提取物进行分离纯化,根据波谱数据结合理化性质解析所得化合物的结构。结果:从牡荆子醋酸乙酯萃取部分分离得到8个化合物,分别鉴定为紫花牡荆素(casticin,1),去四氢铁杉脂素(detetrahydroconidendrin,2),6-羟基-4β-(4-羟基-3-甲氧基苯基)-3α-羟甲基-7-甲氧基-3,4-二氢-2-萘醛(6-hydroxy-4β-(4-hydroxy-3-methoxyphenyl)-3α-hydroxymethyl-7-methoxy-3,4-dihydro-2-naphthaldehyde,3),对羟基苯甲酸乙酯(ethyl p-hydroxybenzoate,4),5,4’-二羟基-3,6,7,8,3’-五甲氧基黄酮(5,4’-dihydroxy-3,6,7,8,3’-pentamethoxyflavone,5),5-羟基-6,7,3’,4’-四甲氧基黄酮(5-hydroxy-6,7,3’,4’-tetramethoxyflavone,6),5,4’-二羟基-6,7,8,3’-四甲氧基黄酮(5,4’-dihydroxy-6,7,8,3’-tetramethoxyflavone,7),异落叶松脂素(isolariciresinol,8)。结论:化合物4,5,7为首次从该属植物中分得,化合物2为首次从该植物中分得。     

小蜡树的酚苷及苯乙醇苷类成分

目的:系统研究小蜡树Fraxinuxsieboldiana枝乙醇提取物的化学成分。方法:运用正相和反相硅胶、大孔吸附树脂、凝胶、反相高效液相等色谱方法进行分离;应用包括一维和二维NMR等波谱方法鉴定化合物的结构。结果:从小蜡树枝的乙醇提取物水相部位分离得到4个酚苷和12个苯乙醇苷类成分,分别鉴定为:2,6-二甲氧基-对苯二酚-4-O-β-D-吡喃葡萄糖苷(1),2,6-二甲氧基-对苯二酚-1-O-β-D-吡喃葡萄糖苷(2),4-羟基-3-甲氧基苯基β-D-吡喃葡萄糖苷(3),4-羟基-3-甲氧基苯基β-D-吡喃木糖基(1→6)-O-β-D-吡喃葡萄糖苷(4),osmanthuside H(5),2-(4-羟基苯基)乙基β-D-吡喃葡萄糖苷(6),2-(3,4-二羟基苯基)乙基β-D-吡喃葡萄糖苷(7),2-羟基-4-(2-羟基乙基)-苯基β-D-吡喃葡萄糖苷(8),4-(2-羟基乙基)-2-甲氧基苯基β-D-吡喃葡萄糖苷(9),calceolarioside B(10),calceolarioside A(11),ferruginoside A(12),isolugrandoside(13),类叶升麻苷(14),chiritotoside C(15)和plantasisoside(16)。结论:化合物1~4,9,12,13和16为首次从该属植物中分离得到。     

漾濞泡核桃青皮中二芳基庚烷类成分研究

综合运用硅胶、Sephadex LH-20、MCI等柱色谱方法对漾濞泡核桃青皮的乙酸乙酯部位化学成分进行了研究,并利用各种波谱技术(MS,~1H-NMR,~(13)C-NMR,2D-NMR)对化合物结构进行了鉴定。结果从乙酸乙酯部位分离得到4个二芳基庚烷类化合物,分别鉴定为:二氢枫杨素(1),1-(4'-羟基苯基)-7-(3″-甲氧基苯基)-3',4″-环氧-3α-庚醇(2),枫杨素(3)和1-(4'-羟基苯基)-7-(3″-甲氧基-4″-羟基苯基)-3α-庚醇(4)。其中,化合物1(二氢枫杨素,dihydropterocarine)为新化合物,化合物2~4首次从该植物中分离得到。     

青龙衣中二芳基庚烷类成分研究

目的:研究青龙衣中具有抗肿瘤活性的二芳基庚烷类成分。方法:采用硅胶柱色谱和大孔吸附树脂等色谱方法对药材抗肿瘤活性部位即乙酸乙酯部位和氯仿部位进行目的性分离。结果:共分离得到5个二芳基庚烷类化合物。利用核磁共振波谱方法确定了化合物的结构,分别为1-(4’-羟基苯基)-7-(3″-甲氧基-4″-羟基苯基)-4-烯-3-庚酮(I),1-(4’-羟基苯基)-7-(3″-甲氧基-4″-羟基苯基)-5-甲氧基-3-庚酮(Ⅱ),1-(4’-羟基苯基)-7-(3″-甲氧基苯基)-2-羟基-3’,4″-环氧-3-庚酮(Ⅲ),4″-epoxy-1-(4’-羟基苯基)-7-(3″-甲氧基苯基)-3’,4″-环氧-3-庚醇(Ⅳ),galleon(V)。结论:其中化合物Ⅰ,Ⅱ为首次从青龙衣中分离得到的线型二芳基庚烷类化合物。     

阿卡如化学成分研究

目的:研究阿卡如的化学成分。方法:采用现代分离方法和色谱技术,对阿卡如乙酸乙酯部位进行分离纯化,采用波谱技术和理化常数对照等方法进行结构鉴定。结果:从阿卡如乙酸乙酯部分分离并鉴定了6个含量相对较高的化合物,分别为3,4-Di-(3-methoxy-4-hydroxyphenyl)tetrahydrofuran(1),开环异落叶松树脂酚(2),3,3'-dimethoxy-8,9-epoxylign-4,4',9'-triol(3),2S,3S,4S-2-羟基-3,4-二-(3,甲氧基-4-羟基苄基)四氢呋喃(4),2-(3,4-次甲二氧基苄基)-3-(3-甲氧基-4-羟基苄基)-1,4-丁二醇(5),2R,3S,4S-2-羟基-3,4-二-(3,4-次甲二氧基苄基)四氢呋喃(6)。结论:首次从该种植物中分离得到化合物1、2、3、5,首次从该植物主干和根中分离得到化合物4和6。     

厚朴水溶性成分分离

目的:研究厚朴的化学成分。方法:采用硅胶,ODS柱色谱,Sephadex LH-20和半制备液相色谱等技术分离纯化,结合ESI-MS,UV,NMR等现代波谱学技术进行结构鉴定。结果:分离并鉴定了9个化合物,分别为(7S,8R)-syringoylglycerol(1),3,4-二羟基-烯丙基苯-3-O-α-L-吡喃鼠李糖(1→2)β-D-吡喃葡萄糖苷(2),3,4-二羟基-烯丙基苯-3-O-α-L-吡喃鼠李糖(1→6)β-D-吡喃葡萄糖苷(3),synapicaldehyde-4-O-β-D-glucopyranoside(4),丁香脂素双葡萄糖苷(5),3,4,5-三甲氧基苯基-β-D-葡萄糖苷(6),厚朴酚(7),和厚朴酚(8),4-O-methylhonokiol(9)。结论:化合物6为首次从厚朴中分离得到。     

鄂西冬凌草化学成分研究

目的对鄂西冬凌草化学成分进行研究。方法运用正相、反相硅胶柱层析和HPLC分离冬凌草叶乙醇提取物,利用现代波谱技术鉴定化合物的结构。结果鄂西冬凌草乙醇提取物中得到7个化合物,分别是冬凌草甲素①,Lasiokaurin②,对羟基苯甲醛③,邻苯二甲酸二丁酯④,5-羟基-3’,4’,6,7-四甲氧基黄酮⑤,5-羟基-3’,4’,7-三甲氧基黄酮⑥,4’,5,7-三甲氧基黄酮⑦。结论 7个化合物均为首次从鄂西地区该植物中分得。     

A New Asymmetric ent-Kauranoid Dimer from Rabdosia rubescens

Objective To study the ent-kaurane diterpenoids from Rabdosia rubescens. Methods The compounds were isolated by chromatographies and their structures were identified by spectral analyses. Results Four compounds were isolated, and they were identified as bisrubescensin E (1), 2α,3α,24-trihydroxyurs-12-en-28-oic acid (2), 2α,3α,24-trihydroxyurs-12,20-(30)-dien-28-oic acid (3), and 6,7-dihydroxycoumarin (4). Conclusion Compound 1 is a new asymmetric ent-kauranoid dimer. Compound 2 is isolated from the plant for the first time. Compounds 3 and 4 are isolated from the plants of Rabdosia (Bl.) Hassk for the first time.     

Highly brominated mono- and bis-phenols from the marine red alga Symphyocladia latiuscula with radical-scavenging activity

Four new highly brominated and fully substituted mono- and bis-phenols, 1-(2,3,6-tribromo-4,5-dihydroxybenzyl)pyrrolidin-2-one (1), 1,2-bis(2,3,6-tribromo-4,5-dihydroxyphenyl)ethane (2), 6-(2,3,6-tribromo-4,5-dihydroxybenzyl)-2,5-dibromo-3,4-dihydroxybenzyl methyl ether (3), and 2,3,6-tribromo-4,5-dihydroxybenzyl methyl sulfone (4), were characterized from the marine red alga Symphyocladia latiuscula. In addition, five known bromophenols, bis(2,3,6-tribromo-4,5-dihydroxyphenyl)methane (5), bis(2,3,6-tribromo-4,5-dihydroxybenzyl) ether (6), 2,3,6-tribromo-4,5-dihydroxybenzyl methyl ether (7), 2,3,6-tribromo-4,5-dihydroxymethylbenzene (8), and 2,3,6-tribromo-4,5-dihydroxybenzaldehyde (9), were also isolated and identified. The structures of these compounds were elucidated by spectroscopic methods including 1D and 2D NMR as well as by low- and high-resolution mass spectrometric analysis. Structurally, all of these compounds are highly brominated and fully substituted, and contain one or two 2,3,6-tribromo-4,5-dihydroxyphenyl unit(s) in each of the molecules. In addition, compound 4 possesses a unique sulfone structural feature. Each of the isolated compounds was evaluated for alpha,alpha-diphenyl-beta-picrylhydrazyl (DPPH) radical-scavenging activity and all were found to be potent, with IC50 values ranging from 8.1 to 24.7 microM, compared to the known positive control butylated hydroxytoluene (BHT), with an IC50 of 81.8 microM.     

Dibenzyl bromophenols with diverse dimerization patterns from the brown alga Leathesia nana

Six novel dibenzyl bromophenols (1-6) with different dimerization patterns and two propyl bromophenol derivatives (7 and 8), together with 11 known bromophenol derivatives, were isolated from the ethanolic extract of the brown alga Leathesia nana. On the basis of spectroscopic methods the structures of the new compounds were determined as 5,6'-diethyloxymethyl-3,4,2'-tribromo-2,3',4'-trihydroxydiphenyl ether (1), 2-(2,3-dibromo-4,5-dihydroxybenzyl)-3,5-dihydroxy-4-methoxybenzyl alcohol (2), 6-(2,3-dibromo-4,5-dihydroxybenzyl)-2,3-dibromo-4,5-dihydroxy benzyl methyl ether (3), 9,10-dihydro-9,10-dimethoxy-3,4,7,8-tetrabromo-1,2,5,6-tetrahydroxyanthracene (4), (+)-3-(2,3-dibromo-4,5-dihydroxyphenyl)-4-bromo-5,6-dihydroxy-1,3-dihydroisobenzofuran (5), rel-(4aS,10aR)-(+/-)-6,7-dibromo-4a-hydroxy-3,8-dihydroxymethyl-10a-methoxy-1,4,4a,10a-tetrahydrodibenzo[b,e][1,4]dioxin-1-one (6), (E)-2-methyl-3-(2,3-dibromo-4,5-dihydroxyphenyl)propenal (7), and 2-methyl-3-(2,3-dibromo-4,5-dihydroxyphenyl)-1-propanol (8). Some compounds including 3 showed in vitro selective cytotoxicity against several human cancer cell lines. This is the first brown alga to be reported containing bromophenols.     

Phenolic compounds from the roots of Jordanian viper's grass, Scorzonera judaica

Nine new phenolic compounds, 3S-hydrangenol 40-O-R-L-rhamnopyranoysl-(1-->3)-β-D-glucopyranoside (1), thunberginol F 7-O-β-D-glucopyranoside (2), 2-hydroxy-6-[2-(4-hydroxyphenyl)-2-oxo-ethyl]benzoic acid (3), 2-hydroxy-6-[2-(3,4-dihydroxyphenyl)-2-oxo-ethyl]benzoic acid (4), 2-hydroxy-6-[2-(3,4-dihydroxyphenyl-5-methoxy)-2-oxoethyl]benzoic acid (5), hydrangeic acid 40-O-β-D-glucopyranoside (6), E-3-(3,4-dihydroxybenzylidene)-5-(3,4-dihydroxyphenyl)dihydrofuran-2-one (7), Z-3-(3,4-dihydroxybenzylidene)-5-(3,4-dihydroxyphenyl)-2(3H)-furanone (8), and 4-[β-D-glucopyranosyl)hydroxy]-pinoresinol (9), and nine known compounds were isolated from the roots of Scorzonera judaica. Structures of 1-9 were elucidated by mass spectrometry, extensive 1D and 2D NMR spectroscopy, and CD spectroscopy.All compounds were evaluated for cytotoxic activity.     

小槐花的化学成分研究

目的:系统研究中药小槐花中的化学成分。方法:利用大孔树脂,Sephadex LH-20,ODS及正相硅胶柱等色谱手段进行分离,通过多种波谱学数据分析进行化合物的结构鉴定。结果:从小槐花60%乙醇提取物中分离得到15个化合物,经结构鉴定分别为豆甾醇(1),β-谷甾醇(2),柠檬酚(3),黄槿酮A(4),异柠檬酚(5),kenusanone I(6),neophellamuretin(7),清酒缸酚(8),古柯三醇(9),黄槿酮D(10),山柰酚(11),8-prenylquercetin(12),leachianone G(13),5,7,4’-三羟基-二氢黄酮醇(14),4H-1-benzopyran-4-one,2-(3,4-dihydroxyphenyl)-2,3-dihydro-3,5,7-trihydroxy-8-(3-methyl-2-butenyl)-,(2R-trans)-(9CI)(15)。结论:除化合物8外,所有化合物均为从该种植物中首次分离得到。     

红药苯乙醇苷类化学成分的研究

目的:分离鉴定红药干燥茎的化学成分。方法:甲醇提取,硅胶、Sephadex LH-20及ODS柱色谱分离,采用NMR和MS等方法确定化合物的结构。结果:分离鉴定了5个苯乙醇苷类化合物,分别为3,4-dihydroxyphenylalcohol-β-D-glucopyranoside(1),3,4-dihydroxyphenyl alcohol-6-O-caffeoyl-β-D-glucopyranoside(calceolarioside B)(2),3,4-di-hydroxyphenyl alcohol-β-D-glucopyranosyl-(1→3)-6-O-caffeoyl-β-D-glucopyranoside(plantainoside D)(3),3,4-dihydroxyphenylalcohol-β-D-glucopyranosyl-(1→3)-4-O-caffeoyl-β-D-glucopyranoside(plantamajoside)(4),3,4-dihydroxyphenyl alcohol-β-D-glucopyranosyl-(1→3)-6-O-feruloyl-β-D-glucopyranoside(scroside E)(5)。结论:化合物3,5为首次从该科植物中得到,化合物1,2,4为首次从该属植物中得到。     

小木通的化学成分

目的:系统研究小木通的化学成分.方法:采用硅胶柱色谱、凝胶柱色谱和中低压制备色谱等技术分离小木通的化学成分,利用理化性质和波谱法鉴定其结构.结果:从小木通中分离得到11个化合物,分别鉴定为4,7-二甲氧基-5-甲基-香豆素(1),异松脂素(2),松脂素(3),(+)-2-(3,4 -dimethoxyphenyl)-6-(3,4-dihydroxyphenyl)-3,7-dioxabicyclo[3,3,0]octane (4),matairesinol (5),落叶松脂素(6),justieiresinol(7),丁香脂素(8),鹅掌楸苷(9),3-甲氧基-对苯二酚-4-O-β-D-葡萄糖苷(10),3,5-二甲氧基-对苯二酚-1-O-β-D-葡萄糖苷(11).结论:除了化合物9外,其余10个化合物均为首次从该植物中分离得到.     

柔茎香茶菜中的二萜化合物

香茶菜属植物富含结构多样、新奇的对映,贝壳杉烷二萜及其衍生物,前期对柔茎香茶菜Rabdosia flexicaulis的化学成分研究尚不够系统,仅从中发现3个这类化合物.为了寻找结构新颖、活性显著的二萜化合物,采集了四川省道孚县的柔茎香茶菜地上部分,采用多种柱色谱法和波谱分析手段,从乙酸乙酯部位中分离并鉴定出6个二萜化...     

Bromophenols from the red alga Rhodomela confervoides

Six new bromophenols, 3-bromo-4,5-bis(2,3-dibromo-4,5-dihydroxybenzyl)pyrocatechol (1), 2,2',3-tribromo-3',4,4',5-tetrahydroxy-6'-hydroxymethyldiphenylmethane (2), 2,2',3-tribromo-3',4,4',5-tetrahydroxy-6'-ethyloxymethyldiphenylmethane (3), (+/-)-2-methyl-3-(2,3-dibromo-4,5-dihydroxyphenyl)propylaldehyde (4), (+/-)-2-methyl-3-(2,3-dibromo-4,5-dihydroxyphenyl)propylaldehyde dimethyl acetal (5), and 3-bromo-4,5-dihydroxybenzoic acid methyl ester (6), together with eight known bromophenols, 3-bromo-4,5-dihydroxybenzaldehyde (7), 2,3-dibromo-4,5-dihydroxybenzyl alcohol (lanosol, 8), 2,3-dibromo-4,5-dihydroxybenzyl methyl ether (9), 2,3-dibromo-4,5-dihydroxybenzyl ethyl ether (10), 2,3-dibromo-4,5-dihydroxybenzylaldehyde (11), bis(2,3-dibromo-4,5-dihydroxybenzyl) ether (12), 3-bromo-4-(2,3-dibromo-4,5-dihydroxybenzyl)-5-methoxymethylpyrocatechol (13), and 2,2',3,3'-tetrabromo-4,4',5,5'-tetrahydroxydiphenyl methane (14), were isolated from the red alga Rhodomela confervoides. Their structures were elucidated by chemical and spectroscopic methods including IR, HRFABMS, and 1D and 2D NMR techniques.