(2′-溴-4′，5′-二甲氧基-苯基)-(2，3-二溴-4，5-二甲氧基-苯基)-甲烷的合成及其PTP1B酶抑制活性研究

目的：通过化学法合成具有PTP1B酶抑制活性的新型溴酚衍生物-(2′-溴-4′,5′-二甲氧基-苯基)-(2,3-二溴-4,5-二甲氧基-苯基)-甲烷。方法：采用傅克酰基化、逐级溴化、脱羰基等经典合成反应合成目标化合物6。采用EI-MS,HREI-MS,1H-NMR,13C-NMR,IR等方法对合成中间体及目标化合物进行结构鉴定。通过比色法对化合物6进行PTP1B酶抑制活性测试。结果：采用四步法成功合成了目标化合物6,体外活性测试结果表明其具有一定的PTP1B酶抑制活性。结论：采用化学法合成了目标化合物6,总产率为20%,该化合物为新化合物,具有一定的PTP1B酶抑制活性5 mg·L-1,酶抑制率为40.16%。     

(2'-溴-4',5'-二甲氧基-苯基)-(2,3-二溴4,5-二甲氧基-苯基)-甲烷的合成及其PTP1B酶抑制活性研究

目的:通过化学法合成具有PTP1 B酶抑制活性的新型溴酚衍生物-(2'-溴4',5'-二甲氧基-苯基)-(2,3-二溴-4,5-二甲氧基-苯基)-甲烷.方法:采用傅克酰基化、逐级溴化、脱羰基等经典合成反应合成目标化合物6.采用EI-Ms,HREI-MS,~(1)H-NMR,~(13)C-NMR,IR等方法对合成中间体及目标化合物进行结构鉴定.通过比色法对化合物6进行PTP1 B酶抑制活性测试.结果:采用四步法成功合成了目标化合物6,体外活性测试结果表明其具有一定的PTP1 B酶抑制活性.结论:采用化学法合成了目标化合物6,总产率为20%,该化合物为新化合物,具有一定的PTP1 B酶抑制活性5 mg·L~(-1),酶抑制率为40.16%.     

高效液相色谱法测定2-(2,6-二氯苯基氨基)苯乙酸-4-(4-苯基-1,2,5-噁二唑-2-氧化物-3-)甲氧基苯甲酯原料药的研究

 目的采用反相高效液相色谱法建立2-(2,6-二氯苯基氨基)苯乙酸-4-(4-苯基-1,2,5-二唑-2-氧化物-3-)甲氧基苯甲酯(ZLR-8)原料药质量控制的方法。方法色谱柱为Lichrospher ODS柱(4.6 mm×250 mm),流动相为甲醇-乙腈-水(55∶20∶10),检测波长为226 nm,流速为1.0 mL·min^-1。结果中间体及各降解产物对样品测定不产生干扰,ZLR-8的浓度为11.18～223.6mg·L^-1时与峰面积呈良好线性关系(r=0.999 8,n=5),重复性良好(RSD%=0.47,n=6),检测限为54μg·L^-1。结论该方法可以用于ZLR-8原料药的含量测定和有关物质检查。     

矮慈姑中新的对映贝壳杉烷二萜

目的：研究矮慈姑（Sagittaria pygmaea Miq）全草中的二萜类成分。方法：采用硅胶柱层析、Sephadex LH-20柱层析等方法进行分离和纯化化学成分，结合化学方法和渡谱学方法进行结构鉴定。结果：从矮慈姑乙醇提取物的石油醚萃取部分中分离得到5个二萜类化合物，包括一个对映贝壳杉烷，为19-β-L-3′-acetoxyarabinofuranosyl-eru-kaur-16-ene（1），3个半日花烷，分别为13-epi-manoyloxide-18-ol（2），13-epi-manoyloxide-18-oic acid（3）和13-epi-manoyl oxide-18-O-α-L-2′，5′-diacetoxyarabinofuranoside（4），一个玫瑰烷为5α-hydroxy-ent-rosa-15-en-19-oic acid（5）。结论：上述化合物均从该属植物中首次得到，其中化合物1为新化合物。     

墨旱莲中一个新的苯甲酸类化合物

目的：对墨旱莲（Eclipta prostrata）地上部分的化学成分进行研究。方法：采用硅胶柱色谱、SephadexLH-20对墨旱莲80%乙醇提取浸膏的乙酸乙酯部分进行分离纯化,并应用波谱方法鉴定其结构。结果：分离鉴定了8个化合物,分别为2,6-二羟基-4-甲氧基苯甲酸乙酯（ethyl2,6-dihydroxy-4-methoxy benzoate）（1）、干朽菌酸C（merulinic acidC）（2）、β-香树酯酮（β-amyrone）（3）、齐墩果酸（oleanolic acid）（4）、旱莲苷A（ecliptasaponinA）（5）、蟛蜞菊内酯（wedelolactone）（6）、去甲基蟛蜞菊内酯（demethylwedelolactone）（7）和槲皮素（quercetin）（8）。结论：化合物1为新化合物,化合物2、3为首次从该属中分得。     

A New Cyano-compound from Rhodiola kirilowii

Objective To study the chemical constituents of Rhodiola kirilowii.Methods The compounds were separated and purified by various chromatographic techniques and their structures were elucidated on the basis of physicochemical properties and spectroscopic methods.Results Five compounds were purified and their structures were identified as 4-(β-D-glucopyranosyloxy)-3-hydroxy-2-(hydroxymethyl)-butanenitrile(1),epicatechin(2), arbutin(3),rutin(4),andβ-D-glucose(5).Conclusion Compound 1 is a new cyano-compound and other compounds are isolated from the plant for the first time.     

南欧大戟中一个新的假白榄烷型二萜

目的：研究南欧大戟全草的化学成分。方法：采用硅胶柱色谱、凝胶柱色谱和MCI等分离纯化化合物,利用ESI-MS,IR,NMR确定化合物的结构。结果：分离鉴定了3个化合物,分别为：euphopeplin A（1）,2α,5α,7β,8α,9α,14β-hexa-acetoxy-3β-benzoyloxy-15-hydroxyjatropha-6（17）,11E-diene（2）和5α,8α,9β,10β,14α-pentaacetoxy-3β-benzoyloxy-15-hydroxy-pepluane（3）。结论：化合物1为一新化合物。     

云南石仙桃中一个新的菲类化合物

 目的分离鉴定云南石仙桃中的化学成分。方法用体积分数为95%乙醇提取,硅胶柱色谱分离,用IR,UV,MS,¹H-NMR,¹³C-NMR和HMBC等方法确定结构。结果分得5个化合物,分别为n-octacostyl ferulate(Ⅰ),β-谷甾醇(β-sitosterol,Ⅱ),batatasin-Ⅲ(Ⅲ),石仙桃菲(pholidotol,Ⅳ)和胡萝卜苷(daucosterol,Ⅴ)。结论石仙桃菲为一新的菲类化合物,其结构确定为1,6-二羟基-2-甲氧基-8,9-二氢-三氢菲[4,5-环]呋喃(1,6-dihydroxy-2-methoxy-8,9-dihydro-3H-phenanthro-[4,5-bcd]furane)。     

A New Prenylated Xanthone from Root Barks of Cudrania cochinchinensis

Objective To study the chemical constituents from the root barks of Cudrania cochinchinensis. Methods The chemical constituents were isolated and purified by silica gel column chromatography. The structures of the compounds were identified on the basis of spectral data(MS,1H-NMR,13C-NMR, and 2D NMR) and by the comparison of spectroscopic data with the reported values in the literatures. Results A new xanthone, 1,6,7-trihydroxy-4-(1,1-dimethylallyl)-3-methoxyxanthone(1) and a known prenylated xanthone 1,5,6-trihydroxy-4-(1,1-dimethylallyl)-3-methoxyxanthone(isocudraniaxanthone B, 2) were isolated from the root barks of C. cochinchinensis. Conclusion Compound 1 is a new prenylated xanthone. Isomers 1 and 2 are obtained from this plant for the first time.     

A New Phenylated Flavone from Melicope pteleifolia

Objective To study the constituents in Melicope pteleifolia.Methods Plant material was isolated with 80% EtOH.Compounds were separated with chromatographic methods and their structures were elucidated on the basis of spectral analysis(EI-MS,1H-NMR,and 13C-NMR) and chemical evidence.Results Five compounds were isolated from petrol ether or ethyl acetate soluble fraction.Their structures were identified as 3,5,3’-trihydroxy-4’-methoxy-7-(3-methylbut-2-enyloxy) flavone(pteleifolosin C,1),3,7-dimethoxyl kaempferol(kamatakenin,2),vanillic acid(3),tricosanoic acid tetradecyl ester(4),and β-sitosterol(5),respectively.Conclusion Compound 1 is a new structure named pteleifolosin C.Compounds 2-4 are isolated from this plant for the first time.     

钩吻吲哚生物碱化学成分研究

目的为了寻找钩吻Gelsemium elegans的活性成分,对其化学成分进行研究。方法运用正反相柱色谱、葡聚糖凝胶等分离技术,根据化合物的波谱数据鉴定化合物的化学结构。结果从乙醇提取物的氯仿萃取部位分得8个化合物,分别鉴定为gelsemoxonmine Ⅱ(1)、koumine(2)、gelsemine Ⅰ(3)、胡蔓藤碱Ⅳ(4)、19-(Z)-koumidine(5)、19-(Z)-akuammidine(6)、4-(R)-gelsemine-N-oxide(7)和4-(S)-gelsemine-N-oxide(8)。结论化合物1～7是首次从采自西双版纳的钩吻地上部分分离得到的钩吻类吲哚生物碱,化合物8为新天然产物。     

红芪中的一个新苯丙酰衍生物

目的：研究红芪（Hedysarum polybotrys）的化学成分。方法：运用各种色谱方法分离化合物,根据理化性质和光谱数据鉴定化合物的结构。结果：从红芪中分离并鉴定得到1个化合物,鉴定为（E）-3-（4-羟基-2-甲氧基）-苯丙烯酸-4-羟基-3-甲氧基苯酯。结论：该化合物为新化合物。     

A New Natural Compound with Cytotoxic Activity from Tripterygium hypoglaucum

Objective To find antitumor constituents from Tripterygium hypoglaucum.Methods The chloroform extract of T.hypoglaucum was separated by silica gel column chromatography and preparative HPLC.The structures of compounds isolated were identified by spectral analysis and chemical evidence.Results Seven compounds were isolated and identified as rhein ethyl ester(1),chrysophenol(2),physcion(3),emodin(4),wilfordine(5),wilforgine(6),and wilforine(7).The cytotoxic activities of the compounds against cancer cell lines were assayed.Conclusion Compound 1 is a new natural compound with strong activities against human cancer cell lines(A2780 and OVCAR-3) .Compounds 2-4 are isolated from this genus plants for the first time.The possible structure-activity relationship among compounds 1-4 shows that the methoxy group or oxyethyl moiety might be responsible for the cytotoxity.