HPLC同时测定黔产红禾麻中4种儿茶素类成分含量

目的:建立HPLC同时测定红禾麻中4种儿茶素类成分含量的方法。方法:采用Diamonsil C18色谱柱(4.6mm×250 mm,5μm),流动相乙腈-0.1%磷酸水溶液梯度洗脱,流速1.0 mL·min-1,检测波长210 nm,柱温35℃。结果:(-)-没食子儿茶素、(±)-表没食子儿茶素、(+)-儿茶素、(-)-表儿茶素线性范围分别为0.050 50~1.010μg(r=0.999 9),0.050 05~1.001μg(r=0.999 9),0.025 75~0.515 0μg(r=0.999 9),0.016 65~0.333 0μg(r=0.999 9);平均加样回收率分别为97.39%,98.45%,99.17%,97.87%。结论:该方法简便、准确、重复性好,可用于红禾麻药材的质量控制。     

八角茴香油精馏釜底残液中1个新的苯甲醛类化合物

目的研究八角茴香油精馏釜底残液的化学成分。方法运用多种色谱方法进行分离纯化,根据理化性质和波谱数据鉴定化合物的结构。结果从八角茴香油精馏釜底残液中得到2个化合物,分别鉴定为(E)-1,4-二(4-甲氧基苯基)-3-丁烯-2-酮(1)和4-羟基-3-(3-甲基-3-丁烯-2-基)苯甲醛(2)。结论化合物1的核磁数据为首次报道,化合物2为新化合物。     

红花中2个倍半萜的分离和鉴定

目的 研究菊科植物红花Carthamus tinctorius的化学成分.方法 通过大孔吸附树脂、硅胶柱色谱、Sephadex LH-2O 色谱以及制备HPLC等方法进行分离纯化,并鉴定化合物的结构.结果 从红花水提部分得到2个倍半萜类化合物,通过波谱学方法分别鉴定为(-)-methyl dihydrophaseate(1)和(-)-(9E)-methyl dihydrophaseate (2).结论 其中化合物2为新化合物,命名为红花酯A.     

羊红膻根中羊红膻素G等的分离和鉴定

目的:对羊红膻根进行降压有效成分的分离和鉴定。方法:采用柱层色谱法进行分离,光谱技术鉴定化合物的结构。结果:从其根中分得3个化合物,2(1′,2′环氧基)丙基4甲氧基苯酚(2″甲基)丁酸酯(Ⅰ),4(1丙烯基)苯酚(Ⅱ),2甲基丁酸(Ⅲ)。结论:Ⅰ为一新化合物,定名为羊红膻素G,Ⅱ,Ⅲ为首次从该植物中分离得到。     

血清葡萄糖-6-磷酸异构酶与类风湿性关节炎相关性研究

目的:探讨血清葡萄糖-6-磷酸异构酶(GPI)水平与类风湿性关节炎(RA)相关性及其对RA的诊断价值。方法:采用酶联免疫吸附试验(ELISA)检测64例RA患者、70例非RA患者包括34例其他自身免疫性疾病(AID)患者(SLE、SS、MCTD等)和36例风湿性关节炎患者、42例健康体检者血清GPI浓度并进行比较。结果:当GPI以0.28μg/ml为临界值时,RA组的GPI阳性率显著高于其他AID组、风湿性关节炎组及健康对照组,阳性率分别为68.7%、26.5%、2.7%、2.4%,RA组的GPI阳性率与其他各组差异有统计学意义(P<0.01)。RA患者中GPI阳性率与类风湿因子(RF)阳性率分别为68.7%和67.2%,GPI和RF单项和/或双项阳性率达93.7%。结论血清GPI在各对照组中,以RA组升高最明显,对RA诊断具有较高的灵敏度和特异性,可作为除RF外诊断RA的新指标,与RF联合检测,可提高RA的诊断率。     

(-)-儿茶素没食子酸酯和(+)-表儿茶素对心肌细胞保护作用研究

目的:观察(-)-儿茶素没食子酸酯[(-)-CG]和( )-表儿茶素[( )-EC]对心肌细胞黄嘌呤/黄嘌呤氧化酶体系损伤的保护作用.方法:建立心肌细胞黄嘌呤/黄嘌呤氧化酶体系损伤模型,倒置显微镜观察加入(-)-CG、( )-EC后细胞形态学变化;噻唑盐比色法测定细胞活性;测定细胞培养液中乳酸脱氢酶(LDH)、丙二醛(MDA)、超氧化物歧化酶(SOD)含量.结果:(-)-CG、( )-EC能够增加心肌细胞存活率,降低心肌细胞LDH的漏出量,增加SOD活性,降低培养液中MDA的含量.结论:(-)-CG、( )-EC具有抗体外培养大鼠乳鼠心肌细胞黄嘌呤/黄嘌呤氧化酶体系损伤的作用.     

穿心草𠮿酮类化学成分及抗炎活性研究

目的 研究穿心草Canscora lucidissima全草中酮类成分。方法 运用硅胶柱色谱、MCI柱色谱、半制备HPLC及重结晶等多种分离方法对穿心草95%乙醇提取物进行分离纯化，根据理化性质以及波谱数据对分离的单体化合物进行结构鉴定，对获得的化合物采用Griess法测定抗炎活性。结果 从穿心草中共分离得到18个化合物，分别为1-羟基-3,5-二甲氧基(口山)酮（1）、1-羟基-3,7-二甲氧基(口山)酮（2）、1,5-二羟基-3-甲氧基(口山)酮（3）、1,3-二羟基-5-甲氧基(口山)酮（4）、1,3,7-三羟基-6-甲氧基(口山)酮（5）、5-羟基-1,3-二甲氧基(口山)酮（6）、1,6-二羟基-3,7-二甲氧基(口山)酮（7）、1,5-二羟基-3,6-二甲氧基(口山)酮（8）、1,3,5-三羟基酮（9）、3,7,8-三羟基-1-甲氧基(口山)酮（10）、1,3,7-三羟基酮（11）、1,3,7,8-四羟基酮（12）、1,3,5,8-四羟基酮（13）、1,3,6-三羟基-5-甲氧基(口山)酮（14）、1,5,6-三羟基-3-甲氧基(口山)酮（15）、1,3,6,7-四羟基酮（...     

竹根化学成分的研究(Ⅱ)

目的 研究竹根的化学成分.方法 采用色谱方法 分离化学成分,根据波谱数据及理化常数分析进行结构鉴定.结果 分离鉴定了9个化合物,分别为3-(p-羟基苯)-(2,3)环氧-1-丙酸(Ⅰ),2,3-二羟基-1-(4-羟基-3,5-二甲氧基苯基)-1-丙酮(Ⅱ)、(+)-鹅掌揪树脂醇B(Ⅲ)、原儿茶醛(Ⅳ)、原儿茶酸(Ⅴ)、荭草苷(Ⅵ)、牡荆苷(Ⅶ)、异荭草苷(Ⅷ)、异牡荆苷(Ⅸ).结论 化合物Ⅰ为新化合物,命名为环氧香豆酸(epoxy coumaric acid).     

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??OBJECTIVE To study the chemical constituents from the stems of Acorus tatarinowii Schott. METHODS The chemical constituents were isolated from the 70% ethanol-soluble extract of the stems of Acorus tatarinowii Schott and purified by a series of column chromatography methods, including MCI, silica gel, Sephadex LH-20, HPLC and so on, and their structures were identified by physical chemical constants and NMR techniques. RESULTS A total of twelve compounds were isolated and identified as(7S,8R)-4,9??-dihydroxyl-3,3??-dimethoxyl-7,8-dihydrobenzofuran-1??-propylneolignan(1),(-)-lyoniresinol(2), dihydrocubebin(3), evofolin B(4),(+)-icariol A₂(5), ??-sitosterol(6),(+)-13-hydroxyspathulenol(7), aromadendrane-4??,10??-diol(8), anomallenodiol(9),(9CI)-cis-4-(3,4-dihydroxy-2,6,6-trimethyl-1-cyclohexen-1-yl)-2-butanone(10),(3E)-rel-4-[(3R,4S)-3,4-dihydroxy-2,6,6-trimethyl-1-cyclohexen-1-yl]-3-buten-2-one(11), and ixerol B(12), respectively. CONCLUSION Compounds 2-4 and 7-12 are isolated from the genus Acorus for the first time, and compound 5 is isolated from this plant for the first time.     

飞机草化学成分研究

目的 研究飞机草Eupatorium odoratum地上部分的化学成分.方法 通过色谱技术进行分离纯化,利用质谱、核磁共振等波谱技术鉴定化合物的结构.结果 从飞机草地上部分分离得到7个木脂素类化合物及6个其他类型化合物,分别鉴定为(-)-松脂素(1)、7-甲氧基松脂素(2)、(-)-橄榄脂素(3)、臭矢菜素C(4)、(-)-杜仲树脂酚(5)、(-)-丁香树脂酚(6)、臭矢菜素A(7)、金色酰胺醇酯(8)、天师酸(9)、β-谷甾醇(10)、3β-乙酰基齐墩果酸(11)、乌苏酸(12)和β-胡萝卜苷(13).结论 化合物1～9、11、12为首次从该属中分离得到,同时化合物1～7也是该属中首次分得的木脂素类化合物.     

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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 study the chemical constituents of Patrinia villosa (Thunb.) Juss. METHODS The compounds were isolated by a combination of various chromatographic techniques including column chromatography over macroporous resin, Sephadex LH-20, and reversed-phase HPLC. Their structures were elucidated by physiochemical property and spectral analysis. RESULTS Eleven compounds were isolated and identified as(7R,8S)-3,3??,5-trimethoxy-4??,7-epoxy-8,5??-neolignan-4,9,9??-triol-9-O-??-D-glucopyranoside(1), massonianoside D(2),(7R,8S)-dihydroxydehydrodiconiferyl alcohol-4-O-??-D-glucopyranoside(3),(7S,8R)-dihydroxydehydrodiconiferyl alcohol-4-O-??-D-glucopyranoside(4), 7R,8S-glochidioboside(5), lariciresinol-4-O-??-D-glucopyranoside(6), lariciresinol-9-O-??-D-glucopyranoside(7), lariciresinol-4??-O-??-D-glucopyranoside(8), tortoside B(9), tanegool(10), and tanegool-7??-methyl ether(11). CONCLUSION All compounds are isolated from Patrinia genus for the first time.     

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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.
     

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??OBJECTIVE To study the chemical constituents from the aerial parts of Paris polyphylla var. chinensis. METHODS The compounds were isolated and purified from the 75% ethanol extract by chromatography on HPD100 macroporous resin, silica gel, and Sephadex LH-20 as well as semi-preparative HPLC. Their structures were elucidated on the basis of spectral data. RESULTS Eleven compounds were isolated and identified as corchionoside C (1), ??-ecdysterone (2), coronatasterone (3), kaempferol-3-O-??-D-galactopyranoside (4), astragalin (5), isorhamnetin-3-O-??-D-glucopyranoside (6), kaempferol-3-O-??-D-glucopyranosyl-(l??2)-??-D-galactopyranoside(7), isorhamnetin-3-O-??-D-glucopyranosyl-(l??2)-??-D-galactopyranoside (8), kaempferol-3-O-??-D-glucopyranosyl-(l??2)-??-D-glucopyranoside (9), isorhamnetin-3-O-??-D-galactopyranosyl-(l??6)-??-D-glucopyranoside (10), and isorhamnetin-3-O-??-D-gentiobioside (11). CONCLUSION Compounds 1 and 3-11 are isolated from this plant for the first time and compounds 1, 3-5 and 8-10 are isolated from Paris plants for the first time.     

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??OBJECTIVE To study the chemical constituents of Yao medicine, Zhongliuteng, the stems of Pileostegia tomentella. METHODS The chemical constituents were isolated and purified by silica gel chromatography repeatedly, and their structures were identified by spectral analysis and chemical METHODS. RESULTS Thirteen compounds were isolated from the stems of P. tomentella and the structures were identified as 1-O-(??-D-glucosyl)-2-[2-methoxy-4-(??-hydroxypropyl) phenoxy]propan-3-ol(1),(+)-lyoniresinol-3a-O-??-D-glucopyranoside (2),syringin (3),coniferin (4),dihydroconiferin (5),but-3-enyl-??-D-glucoside (6),4-(2,3-dihydroxypropyl)-2,6-dimethoxy phenyl ??-D-glucopyranoside (7),nikoenoside (8),protocatechuic acid ethyl ester (9),8-methoxy coumarin-7-O-??-D-glucopyranoside (10),6-O-R-L-rhamnopyranosyl-??-D-glucopyranoside methyl salicylate (11), nicotinamide (12), and 3,5-di-O-caffeoyl quinicacid methyl ester (13). CONCLUSION All compounds were obtained from the genus 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 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 study the chemical constituents of Magnolia biondii.Pamp. METHODS The compounds were isolated and purified by Diaion HP-20, Toyopearl HW-40, silica gel column chromatography and semi-preparative HPLC and so on. The structures were elucidated on the basis of spectral data and physiochemical properties. RESULTS Fourteen compounds were isolated and identified as 4-O-??-D-glucopyranosylvanillic acid(1), tachinoside(2), methyl 4-hydroxy-3-methoxybenzoate(3), caffeic acid(4), 3,4,5-trimethoxyphenyl-??-D-glucopyranoside(5), benzyl-O-??-D-glucopyranoside(6), benzyl-O-??-D-galactopyranoside(7), syringin(8), vanillic acid glucosyl ester(9), vanillic acid(10), 1??-(3,4-dihydroxycinnamoyl)cyclopentane-2??,3??-diol(11), scopolin(12),7-methoxycoumarin-6-O-??-D-glucopyranoside(13), and scopoletin(14). CONCLUSION Compounds 1-9 and 11-13 are isolated from this plant for the first time.     

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??OBJECTIVE To study the chemical constituents from the fruits of Lycium ruthenicum Murr. METHODS The compounds were isolated by various chromatographic METHODS including macroporous adsorption resin, silica gel, ODS, Sephadex LH-20 column chromatography, and preparative HPLC, and their structures were elucidated on the basis of spectroscopic data and physico-chemical METHODS. RESULTS Eleven compounds were isolated from the 65% ethanol extract of the fruits of Lycium ruthenicun Murr., and their structures were identified as p-hydroxyphenethyl trans-ferulate(1), kaempferol 3-O-??-D-glucopyranoside(2), quercetin 3-O-??-D-glucopyranoside(3), syringin(4), quercetin(5), ethyl caffeate(6), p-coumaric acid(7), ferulic acid(8), 2,6-bis(1-phenylethyl) phenol(9), dotriacontane(10), and daucosterol(11). CONCLUSION Compounds 1-4, 6, 9, and 10 are for the first time isolated from Lycium ruthenicum Murr. Compounds 1-8 show moderate protective effects on OGD-induced PC12 cell lines.