檵木水溶性化学成分研究

目的 研究檵木水溶性化学成分。方法 采用大孔树脂、硅胶、凝胶、制备高效液相等色谱技术进行分离,根据波谱数据对化合物进行结构鉴定。结果 从檵木叶中分离得到10个化合物,分别鉴定为(6S,9R)-roseoside(1),rhododendrin(2),epirhododendrin(3),(1S,2R,4S,5S)(-)-Angelicoidenol 2-O-β-D-glucopyranoside(4),dihydroalangionoside A(5),(Z)-3-hexenyl β-primeveroside(6),benzyl β-primeveroside(7),(Z)-3-hexenyl O-α-L-rhamnopyranosyl-(1→6)-β-D-glucopyranoside(8),rhododendrol 4'-O-β-D-glucopyranoside(9),3-(4-hydroxyphenol)propyl β-D-glucopyranoside(10)。结论 化合物1~7,9,10均首次从该属植物中分离得到。     

百两金根的化学成分研究

目的 百两金为传统苗药,其化学成分的有关研究报道较少,本研究目的在于研究百两金的化学成分。方法 将百两金干燥根体积分数70%乙醇提取物利用硅胶、重结晶、ODS及制备/半制备HPLC进行分离纯化,根据理化性质及波谱数据对所得化合物结构进行鉴定。结果 从百两金根中得到了20个化合物。分别为岩白菜素 (1)、甲基岩白菜素 (2)、11-O-没食子酰岩白菜素 (3)、 syringin (4)、(+)-syringaresinol-O-β-D-glucopyranoside (5)、(-)-(7R,8S,7′R,8′S)-4,9,4′,9′-tetrahydroxy-3,3′-dimethoxy-7,7′-epoxylignan-9-O-β-D-xylopyranoside (6)、saracoside (7)、isolariciresinol-4-O-β-D-glucopyranoside (8)、(7S,8R)-urolignoside (9)、staphylionoside D (10)、蚱蜢酮 (11)、l-borneol 6-O-β-D-aiosyl-β-D-glucoside (12)、(+)-angelicoidenol 2-O-β-D-glucopyranoside (13)、牡荆素-2″-O-鼠李糖苷 (14)、根皮苷 (15)、phenethyl alcohol β-D-(2′-O-β-D-glucopyranosyl)glucopyranoside (16)、phenylethyl-β-D-glucopyranoside (17)、菖蒲碱C (18)、己内酰胺 (19)、蔗糖 (20)。结论 其中化合物5~19为首次从紫金牛科植物中分离得到,化合物4为首次从紫金牛属植物中分离得到,化合物2和3为首次从该植物中分离得到。其中化合物6是自国内学者2013年从岭南杜鹃分离得到以来第二次被分离得到。     

长叶纽子果根化学成分的研究

目的 研究长叶纽子果根(Ardisia virens Kurz var. annamensis Pitard.)的化学成分。方法 长叶纽子果根体积分数70%乙醇提取物采用硅胶柱、Sephadex LH-20、ODS、制备液相进行分离纯化,根据波谱信息鉴定所得化合物的结构。结果 在长叶纽子果根中分离得到10个化合物,分别鉴定为11-O-咖啡酸岩白菜素(1)、11-O-(3',4'-二甲基没食子酰基)岩白菜素(2)、11-O-乙酰岩白菜素(3)、岩白菜素-11-O-α-D-半乳吡喃糖苷(4)、百两金皂苷B(5)、朱砂根皂苷D(6)、朱砂根皂苷G(7)、(+)-丁香树脂酚(8)、丁香酸(9)、十八碳癸二烯酸-2,3-二羟丙基酯(10)。结论 化合物1~10为首次从该植物中分离得到。     

黄花中华苦荬菜化学成分研究

目的 研究干燥黄花中华苦荬菜全草的化学成分。方法 采用硅胶柱色谱、HPLC、重结晶等方法进行分离纯化,依据理化性质和波谱数据鉴定结构。结果 从黄花中华苦荬菜全草中分离得到15 个化合物,分别鉴定为chinensioide F(1),chinensioide C(2),胡萝卜苷(3),6′-对羟基苯乙酰基-ixerin D(4),对羟基苯乙酸甲酯(5),对羟基苯乙醇(6),3,5-二甲氧基-4-羟基苯丙醇(7),10α-羟基-愈创木烷-12,6-内酯-3-酮(8),β-谷甾醇(9),chinensioide E(10),chinensioide D(11),ixerochinoside(12),3β,10α-二羟基-4(15),11(13)-愈创木二烯-12,6-内酯(13),10α-羟基-11βH-4(15)-愈创木烯-12,6-内酯(14),木犀草素-7-O-β-D-葡萄糖苷(15)。结论 化合物1为新化合物,命名为chinensiode F,4~7、12~14首次从该植物中分离得到。     

蛹虫草活性成分的提取分离及体外抗氧化作用研究

目的 以抑制蛋白酪氨酸磷酸酶1B(PTP1B)活性为导向,筛选蛹虫草子实体有效部位,分离纯化单体化合物,并检测其体外抗氧化作用。方法 通过硅胶色谱柱,半制备高效液相等色谱技术对蛹虫草子实体进行分离纯化,检测各组分对PTP1B的抑制活性;应用核磁碳谱、氢谱数据分析鉴定单体化合物结构;利用MTT法检测单体化合物对PC12细胞的增殖作用,及其对过氧化氢(H₂O₂)损伤的PC12细胞存活率的影响,试剂盒检测单体化合物对细胞乳酸脱氢酶(LDH)、超氧化物歧化酶(SOD)活性及丙二醛(MDA)含量的影响。结果 发现5个对PTP1B具有较强抑制作用的活性成分,将其中活性最高的成分进一步分离纯化,获得单体化合物,经鉴定为β-D-吡喃葡萄糖基-9-甲基-4,8鞘氨醇(5),其对PTP1B具有较强的抑制活性,半抑制浓度(IC₅₀)为(3.42±0.59) μmol·L^-1。该单体化合物对H₂O₂诱导的PC12细胞氧化损伤具有明显的保护作用。结论 首次以抑制PTP1B活性为导向,在蛹虫草中分离得到脑苷脂类单体化合物,其具有抑制PTP1B作用和体外抗氧化活性,为蛹虫草用于糖尿病的预防和治疗奠定理论基础。     

蒙药菟儿丝的化学成分研究

目的 研究蒙药菟儿丝的化学成分。方法 采用硅胶、LH-20柱色谱法及制备高效液相色谱法等分离手段,通过运用各种波谱法和标准品对照法鉴定分离所的化合物。结果 分离鉴定了10个黄酮类化合物,分别为5,3′-二羟基-3,6,7,4′-四甲氧基黄酮（1）,5,3′-二羟基-6,7,4′-三甲氧基黄酮（2）,5,7,3′-三羟基-6,4′-二甲氧基黄酮（3）,槲皮素（4）,金丝桃苷（5）,山柰酚（6）,5,7,3′-三羟基-4′-甲氧基黄酮（7）,木犀草素（8）,3-甲氧基-木犀草素-4′-O-β-D-葡萄糖苷（9）,木犀草素-7-O-β-D-葡萄糖苷（10）。结论 化合物1、2、3、7、9和10为首次该植物中分得。     

替尼类药物关键中间体N-芳基喹唑啉-4-胺化合物的简便合成

目的 研究替尼类药物的关键中间体N-芳基喹唑啉-4-胺化合物的新合成方法,优化反应条件,确定反应底物适用性,推测反应可能机理。方法 以取代邻氨基苯甲腈(1a～1e)和芳胺(2a～2e)为原料,甲酸为反应底物和溶剂,Cu(OTf)₂为催化剂,发生多组分串联反应一锅合成N-芳基喹唑啉-4-胺化合物(3a～3g),考察催化剂及用量、溶剂、反应物用量、反应温度和反应时间对反应的影响。结果 在Cu(OTf)₂的催化下,取代邻氨基苯甲腈、芳胺和甲酸能顺利发生串联的加成/缩合/环化反应,在取代邻氨基苯甲腈5 mmol,芳胺6 mmol,Cu(OTf)₂ 0.5 mmol,甲酸20 mL,110 ℃反应12 h的条件下,以80%～95%的收率得到7个N-芳基喹唑啉-4-胺化合物,目标产物结构经¹H-NMR和¹³C-NMR确证。结论 该方法为合成替尼类药物关键中间体N-芳基喹唑啉-4-胺化合物提供了一种高效简便的绿色工艺,反应条件温和,产物收率高,操作安全简便,对环境友好。     

甘草次酸18位差向异构体对Caco-2细胞P-糖蛋白功能和表达的影响

目的 研究甘草次酸18位差向异构体即18α-甘草次酸、18β-甘草次酸对Caco-2细胞上P-糖蛋白功能和表达的影响。方法 建立Caco-2细胞模型,采用罗丹明-123摄取法评价P-糖蛋白的功能;使用荧光定量PCR检测MDR1 mRNA; Western blot分析Caco-2细胞膜上P-糖蛋白的表达。结果 中、高浓度(1, 10 μmol·L)的18α-甘草次酸和高浓度(10 μmol·L)的18β-甘草次酸使细胞内罗丹明-123摄取减少。高浓度(10 μmol·L)的18α-甘草次酸在转录水平上调MDR1 mRNA的表达;实验浓度的18β-甘草次酸未影响MDR1 mRNA的表达;高浓度（10 μmol·L）18α-甘草次酸对P-糖蛋白有诱导作用,实验浓度的18β-甘草次酸没有影响P-糖蛋白表达。结论 18α-甘草次酸对P-糖蛋白功能和表达的影响均表现为诱导作用,而18β-甘草次酸只对P-糖蛋白功能表现出一定的诱导作用。     

狼毒大戟根中的萜类成分研究

目的:研究狼毒大戟Euphorbia fischeriana根中的萜类成分。方法:利用硅胶、MCI、ODS、Sephadex LH-20柱色谱及半制备高效液相色谱法(HPLC)等分离手段对狼毒大戟根中的萜类成分进行分离纯化,根据理化性质、波谱学数据分析鉴定化合物结构。结果:从狼毒大戟根的80%丙酮提取物中分离鉴定了7个萜类化合物,包括5个二萜类化合物和2个三萜类化合物,分别鉴定为7-羰基脱氢松香酸(1)、trogopteroid F(2)、陶塔二酚(3)、18-羟基弥罗松酚(4)、19-羟基弥罗松酚(5)、环木波罗-22-烯-3β,25-二醇(6)和羽扇豆醇(7)。结论:除了化合物6和7,其余化合物均为首次从狼毒大戟中分离得到。     

狼毒大戟的化学成分研究(Ⅱ)

狼毒大戟Euphorbia fischeriana Steud．系大戟科植物，近年临床多用于治疗肿瘤、皮肤病和结核病等。作者对狼毒大戟的化学成分进行了系统研究。本研究从狼毒大戟石油醚和乙醚萃取物中分离出3个化合物：3，3′-二乙酰基-4，4′-二甲氧基2，2′，6，6′-四羟基二苯基甲烷(Ⅰ)、富马酸(Ⅱ)和β-     

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??OBJECTIVE To study the chemical constituents of the aqueous extract from the aerial part of Sibiraea angustata. METHODS The constituents were isolated by various chromatographic techniques(HP-20 macroporous absorption resin, Sephadex LH-20 gel, Reverse-phase silical gel and PHPLC) and their structures were determined on the basis of physicochemical properties and their spectroscopic data, as well as the literatures. RESULTS Twelve compounds were separated and identified as veratric acid(1),(+)-cycloolivil(2), 3,7-dimethyl-3(E)-6-octadien-5-one-1-O-??-D-glucoside(3), 3,7-dimethyl-3(Z)-6-octadien-5-one-1-O-??-D-glucoside(4), 1-O-??-D-glucopyranosyl(1??2)-??-D-glucopyranosyl-3,7-dimethyl-2(E)-6-heptdiene(5),(7R,8S)-dihydrodehydrodiconiferyl alcohol-9??-O-??-D-glucopyranoside(6),(+)-1-hydroxypinoresinol-1-??-D-glucoside(7), skimmin(8), kaempferol 3-O-??-L-arabinopyranosyl-(1??6)-??-D-galactopyranoside(9), isorhamnetin-3-O-??-D-galactopyranosyl(1??6)-??-D-glucopyranoside(10), isorhamnetin 3-O-??-arabinopyranosyl-(1??6)-??-galactopyranoside(11), and quercetin 3-O-[2''-O-(E)-caffeoyl]-??-L-arabinopyranosyl-(1??6)-??-D-galactopyranoside(12). CONCLUSION All compounds are obtained from the genus of Sibiraea for the first time.     

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??OBJECTIVE To study the flavonoid glycosides of Urena lobata. METHODS Compounds were isolated and purified using various column chromatographies such as D101 macroporous adsorption resin, silica gel, Sephadex LH-20, and prep HPLC. Their structures were identified on the basis of their physicochemical properties and various spectroscopic experiments, including HRESIMS, ¹H-NMR, ¹³C-NMR, HSQC, and HMBC. RESULTS Ten flavonoid glycosides were obtained from the n-BuOH extract of U. lobata including quercetin-3-O-??-D-glucopyranosyl-(1??2)-??-D-galactopyranoside(1), kaempferol-3-O-??-D-glucopyranosyl-(1??2)-??-D-glucopyranosyl-7-O-??-L-rhamnopyranoside(2), quercetin-3-O-??-D-apiofuranosyl-(1??2)-??-D-glucopyranosyl-7-O-??-L-rhamnopyranoside(3), kaempferol-4'-O-??-D-apiofuranosyl-3-O-??-D-glucopyranosyl-7-O-??-L-rhamnopyranoside(4), kaempferol-3-O-??-D-apiofuranosyl-(1??2)-??-D-glucopyranosyl-7-O-??-L-rhamnopyranoside(5), quercetin-3-O-??-D-glucopyranosyl-7-O-??-L-rhamnopyranoside(6), quercetin-3-O-??-D-glucopyranosyl-(1??2)-??-D-glucopyranoside(7), kaempferol-3-O-??-L-rhamnopyranosyl-(1??6)-??-D-glucopyranosyl-(1??2)-??-D-glucopyranoside(8), kaempferol-3-O-??-D-glucopyranosyl-(1??2)-[??-L-rhamnopyranosyl-(1??6)]-??-D-glucopyranoside(9) and kaempferol-3-O-??-D-glucopyranosyl-(1??2)-??-D-glucopyranoside(10). CONCLUSION Compounds 1-3 and 6-10 are firstly obtained from U. lobata.     

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??OBJECTIVE To isolate the chemical constituents from Caulophyllum robustum and confirm their chemical structures. METHODS The chemical constituents were isolated by MCI gel, repeated silica gel chromatography, preparative liquid chromatography.and their structures were elucidated by NMR and MS etc. RESULTS The structures of compounds 1-10 were identified as echinocystic acid (1), oleanolic acid-3-O-??-D-glucopyranosyl-(1??2)-??-L-arabinopyranoside (2), hederagenin-3-O-??-D-glucopyranosyl-(1??3)-??-L-arabinopyranoside (3), hederagenin-3-O-??-D-glucopyranosyl-(1??2) [??-D-glucopyranosyl-(1??3)]-??-L-arabinopyranoside (4), 3-O-??-D-glucopyranosyl-(1??2)-??-L-arabinopyranosyl echinocystic acid-28-O-??-L-rhamnopyranosyl-(1??4)-??-D-glucopyranosyl-(1??6)-??-D-glucopyranosyl ester (5), 3-O-??-L-arabinopyranosyl hederagenin-28-O-(4-O-acetyl)-??-L-rhamnopyranosyl-(1??4)-??-D-glucopyranosyl-(1??6)-??-D-glucopyranosyl ester (6), (6R, 7E, 9R)-9-hydroxy-4, 7-megastigmadien-3-one-9-O-??-D-glucoside (7), (9R)-9-hydroxy-4, 6-megastigmadien-3-one-9-O-??-D-glucoside (8), maltose (9), and sucrose (10). CONCLUSION Compounds 1-10 are firstly isolated from the genus Caulophyllum except 5.     

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??OBJECTIVE To investigate the liposoluble constituents of Urticae Rhizoma. METHODS The compounds were isolated and purified by silica gel, Sephadex LH-20, ODS gel column chromatographies, and semi-preparative HPLC. The structures were elucidated on the basis of spectral data and physiochemical properties. RESULTS Twenty-one compounds were isolated from the ethyl acetate fraction of Urticae Rhizoma, and identified as(-)-urticol(1),(-)-secoisolariciresinol(2), 23-hydroxybetulinic acid(3), 2??,3??, 24-trihydroxy-12-oleanen-28-oic acid(4), cleomiscosin A (5), dihydro-4-hydroxy-5-hydroxymethyl-2(3H)-furanone(6), methyl chlorogenate(7), kaempferol(8), pinoresinol monomethyether-4??-O-??-D-glucopyranoside(9), martairesinol-4??-O-??-D-glucopyranoside(10), cycloolivil-6-O-??-D-glucopyranoside(11), stigmasterol-3-O-??-D-glucopyranoside(12), nicotinamide(13), trans-caffeic acid-4-O-??-D-glucopyranoside(14), esculin(15), 5-hydroxyl-7-methoxycoumarin-8-O-??-D-glucopyranoside(16), 6-oxymethyluteolin-7-O-??-D-glucopyranoside(17), luteolin-7-O-??-D-glucopyranoside(18), quercetin-3-O-(4??-methoxy)-??-L-rhamnopyranoside(19), 2??-deoxy uridine(20), and apigenin-6, 8-di-C-??-D-glycoside(21), respectively. CONCLUSION All the compounds, except 8 and 12, are isolated from U. fissa for the first time. Meanwhile, compounds 5, 6, 9, 10, 11, 14, 16, 17, and 19 are all found in Urticaeae plants for the first time.     

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??OBJECTIVE To investigate the chemical constituents of the aerial parts of Ribes diacanthum Pall. METHODS The compounds were isolated and purified by silica gel, Sephadex LH-20 colunm chromatography and HPLC. The structures were elucidated on the basis of spectral data and physiochemical properties. RESULTS Nineteen compounds were isolated from 95% ethanol extracts and identified as quercetin (1), quercetin-3-O-??-D-glucopyranoside (2), quercetin-3-O-??-L-rhamnopyranoside (3), quercetin-3-O-??-D-neohesperoside (4), mearnsetin (5), myricetin-3-O-??-L-rhamnoside (6), myricetin-3-O-??-D-glucopyranoside (7), mearnsetin 3-O-??-D-glucopyranoside (8), mearnsetin 3-O-??-L-rhamnopyranoside (9), kaempferol-3-O-??-D-glucopyranoside (10), kaempferol 3-O-??-D-(2-O-??-L-rhamnopyranosyl) glucopyranoside (11), kaempferol 3-(2??,6??-di-O-??-L-rhamnosyl)-??-D-glucoside (12), 1,2,4-trihydroxybenzene (13), vanillic acid (14), protocatechuic acid (15), 4-hydroxy benzoic acid (16), gallic acid (17), blumenol C glucoside (18), conocarpan (19). CONCLUSION All the compounds are isolated from the title plant and the NMR data for 8 is reported here for the first time.     

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??OBJECTIVE To investigate the chemical constituents from the stems of Lythrum salicaria L..METHODS The constituents were isolated and purified by silica gel, Sephadex LH-20 column chromatography, and TLC. The structures were identified on the basis of spectral data and physiochemical characteristics. RESULTS Twenty compounds were isolated from 70% ethanol extracts and identified as betulinic acid(1), 2??,3??,24-trihydroxy-12(13)-en-urs-28-oic acid(2), 6-O-(E)- sinapoylpoligalitol(3), feruloyl-6??-O-??-D-glucopyranoside(4), 7-oxo-??-sitosterol(5), en-tisolariciresinol(6), muramine(7), aesculetin(8), apigenin(9),(2E,6S)-2,6-dimethyl-6-O-??-D-xylpyranosyloxy-2,7-menthiafolic acid(10), quercetin3-O-(6??-caffeoyl)-??-D-galactopyranoside(11), cycloart-23-ene-3??,25-diol(12), (1??S,6??R)-8??-hydroxyabscisic acid-??-D-glucoside(13), 3??,5-dihydroxy-3,6,4??-trimethoxyl-7-O-??-D-glucopyranoside flavonoid(14), aurantiamide acetate(15), 5,6,3??,4??-tetrahydroxy-3,7-dimethoxy-flavone(16), ursolic acid(17), oleanolic acid(18), 4-O-11-methyl-oleoside-p-hydroxyphenyl-(6??-11-methyloleoside)-??-D-glucopyranoside(19), and 6-O-galloylarbutin(20). CONCLUSION Except for compounds 8 and 9, all the compounds were isolated from this plant material for the first time.
     

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??OBJECTIVE To study the chemical constituents in the flowers of Chrysanthemum morifolium Ramat. METHODS The compounds were isolated with Diaion HP-20, Toyopearl HW-40, Sephadex LH-20, silica gel column chromatography and preparative HPLC. The structures of the compounds were identified by physiochemical properties and spectral analysis. RESULTS Twenty compounds were obtained, and their structures were identified as luteolin (1), apigenin (2), acacetin (3), diosmetin (4), acacetin 7-O-??-D-glucoside (5), acacetin 7-O-??-D-glucoside (6), acacetin7-O-(6??-O-acetyl)-??-D-glucoside (7), eriodictyol (8), naringenin (9), artemetin (10), 5-hydroxy-6,7,3??,4??-tetramethoxyflavone (11), 5,7-dihydroxy-3??,4??-dimethoxyflavone (12), 4??-methoxyctricin (13), 3??,5??-dimethoxy-4??,5,7-trihydroxyflavone (14), 5,6-dihydroxy-3,7,3??,4??-tetramethoxyflavone (15), luteolin 7-O-??-D-glucuronide methyle ester (16), dihydroquercetin-7-??-D-glucoside (17), quercetin 3-O-??-D-glucoside(18), quercetin 3-O-??-D-glucoside (19), and acacetin 7-O-??-(6??-(E)-crotonylglucopyranoside) (20). CONCLUSION Compounds 9-20 were isolated for the first time from this plant.     

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??OBJECTIVE To investigate the chemical constituents from the stems of Viola japonica var. stenopetala Franch. ex H.METHODS The constituents were isolated and purified by silica gel, Sephadex LH-20 column chromatography, and preparative TLC. The structures were identified on the basis of spectral data and physiochemical characteristics. RESULTS Fifteen compounds were isolated from 70% ethanol extract of Viola japonica var. stenopetala Franch. ex H. and identified as ??-sitosterol (1), daucosterol(2), chlorogenic acid (3), 7-hydroxycoumarin (4), stigmastero-3-O-??-D-glucopyranoside (5), dehydrololiolide (6), kaempferol-7-O-??-D-glucopyranoside (7), characterizedas(+)-pinoresinol-O-??-D-glucopyranoside (8), 5,7-dihydroxy-3,6-dimethoxyflavone (9), apigenin-7-O-??-D-glucoside (10), chryseriol (11), ??-amyrin(12), robinin(13), kaempferol-3,7-di-O-??-L-rahmnoside(14), and solagenin-6-O-??-D-quinovopyranoside(15). CONCLUSION Compounds 8 and 15 are isolated from the plants in Gnaphalium L. for the first time. Compounds 5, 6, 8, 11, 14, and 15 are isolated from this plant material for the first time.