土壤真菌07-11号菌株中的酚酸性成分

以稻瘟霉 (Pyriculariaoryzae)分生孢子及菌丝形态变化为指标 ,对从云南土壤中分离得到0 7 1 1真菌的发酵产物中活性成分追踪分离 ,从其乙酸乙酯层浸膏中得到 3个酚酸性成分 ,经光谱数据分析和理化鉴别 ,分别鉴定为邻羟基苯甲酸 (Ⅰ )、4 ,6 二羟基 5 甲基异苯并呋喃酮 (Ⅱ )及 2 甲酰基 3 ,5 二羟基 4 甲基苯甲酸 (Ⅲ ) ,它们对稻瘟霉分生孢子及菌丝体都有一定抑制作用     

黑黏座孢霉二次代谢产物的两个活性成分

目的研究云南省西双版纳采集的土样中黑黏座孢霉(Myrothecium roridumTode ex Fr.)发酵液的活性成分。方法通过硅胶柱色谱、制备薄层色谱、HPLC等手段进行分离纯化,并根据理化性质和光谱数据鉴定其化学结构。结果从黑黏座孢霉发酵液乙酸乙酯提取物中共分离得到2个化合物,经鉴定分别为黏液霉素A(verrucarin A)和黏液霉素J(verrucarin J),并利用稻瘟霉(Pyricu-laria oryzae)菌丝体形态变化作为活性指标,测定了它们的活性。结论黏液霉素A和J为首次从该菌种中分离得到。     

高效液相色谱法测定肤霉净中苯甲酸和水杨酸的含量

目的:建立肤霉净中两种主要成分苯甲酸和水杨酸的含量测定方法,以控制其质量。方法:采用高效液相色谱法测定。色谱柱为DiscoveryC18柱(250mm×4.6mm,5μm),流动相为甲醇-1%冰醋酸(45∶55),检测波长为230nm,流速为1.0mL/min。结果:苯甲酸的线性范围为0.06704～0.8045μg(r=1.000),水杨酸的线性范围为0.07767～0.9321μg(r=0.9997);平均回收率苯甲酸为98.8%,RSD=1.07%(n=6),水杨酸为99.0%,RSD=1.65%(n=6)。结论:建立了同时对肤霉净中苯甲酸和水杨酸的含量测定方法,该方法快速准确,重现性好。     

石南藤化学成分研究

目的对石南藤Piper wallichii化学成分进行研究。方法应用硅胶、葡聚糖凝胶等色谱技术分离纯化,应用波谱技术确定化合物的结构。结果从石南藤中分离得到了5个化合物,分别为piperlonguminine(trans,trans)(1),4-羟基-3,5-二甲氧基-苯甲酸(2),galgravin(3),β-谷甾醇(4)以及胡萝卜苷(5)。结论五个化合物均为首次从石南藤中得到,化合物1~3为首次从胡椒属中得到。     

微紫青霉中的化学成分研究

目的：研究微紫青霉代谢产物对稻瘟霉分生孢子和菌丝体的生长抑制作用。方法：通过理化性质和光谱数据的分析鉴定结构，利用稻瘟霉模型测试活性。结果与结论：从微紫青霉代谢产物中分离得到了4个化合物，分别鉴定为3-(1-甲基乙基)-6-(1-甲基丙基)-2，5-哌嗪二酮（Ⅰ）、（3S，8аS）-3-甲基-1，2，3，4，6，7，8，8а-八氢吡咯骈[1，2а]-吡嗪-1，4-二酮（Ⅱ）、二十二烷酸（Ⅲ）、2-甲酰基-3，5-二羟基-4-甲基苯甲酸（Ⅳ）。上述4个化合物均对稻瘟霉分生孢子和菌丝体的生长有一定的抑制作用。     

海洋细菌Bacillus sp.发酵液中的化学成分

目的 研究海洋细菌Bncillus sp．发酵液中的化学成分，研究其成分对稻瘟霉的抑制作用，为从海洋微生物代谢产物中寻找新型抗肿瘤、抗真菌活性物质奠定基础。方法 利用各种色谱技术进行分离，根据光谱数据鉴定结构。结果 从中分离得到4个成分，分别鉴定为吡咯并[1，2α]哌嗪-3，6-二酮(I)、尿素(Ⅱ)、苯乙酸(Ⅲ)、3-甲基-2，5-哌嗪二酮(Ⅳ)。结论 化合物I、Ⅲ、Ⅳ对稻瘟霉分生孢子或菌丝体有一定的抑制作用；化合物I、Ⅳ为首次从本属菌种发酵液中分离得到。     

海洋真菌09-1-1-1次级代谢产物的研究

目的从海洋真菌的代谢产物中寻找新的具有抗真菌活性的化合物。方法以稻瘟霉生物模型筛选海洋真菌,获得编号09-1-1-1的活性菌株,从其发酵液中分离活性代谢产物。结果从发酵液中分离到2个化合物,鉴定其结构为3a,12c-二氢-8-羟基-6-甲氧基-7H-呋喃[3′,2′∶4,5]呋喃[2,3-c]呫吨-7-酮(Ⅰ,sterig-matocystin)和1,3,6,8-四羟基-2-(1-羟己基)-9,10-蒽二酮(Ⅱ,averantin)。结论稻瘟霉生物模型用于筛选海洋真菌活性代谢产物成本低、快速又方便。化合物Ⅱ对109稻瘟霉菌丝的生长最小抑制浓度为1.6μg.mL-1。     

海洋细菌Bacillus sp.发酵液中化学成分的研究

目的：研究海洋细菌Bacillus sp．菌株发酵液的化学成分．研究其成分对稻瘟霉的抑制情况．为从海洋微生物代谢产物中寻找新型抗肿瘤、抗真菌活性物质奠定基础。方法：利用各种色谱层析技术进行分离．根据光谱数据鉴定其结构。结果：从中分离得到8个成分．分别鉴定为吡咯并哌嗪2，5-二酮(Ⅰ)、3-异丁基-吡咯并哌嗪2，5-二酮(Ⅱ)、3-甲基-哌嗪-2，5-二酮(Ⅲ)、胸腺嘧啶(Ⅳ)、尿嘧啶(Ⅴ)、曲酸(Ⅵ)、丁四醇(Ⅶ)、苯丙氨酸(Ⅷ)。结论：其中化合物Ⅰ，Ⅱ，Ⅲ对稻瘟霉分生孢子或菌丝体有一定抑制作用；化合物Ⅵ为首次从本属菌中分离得到。     

桑椹的化学成分

目的对桑科植物桑 (MorusalbaL .)的果实桑椹醇提取物中的化学成分进行提取分离和结构鉴定。方法色谱技术进行分离 ,MS、NMR和IR光谱解析及与对照品比较鉴定化合物。结果共分离得到 7个化合物 ,根据理化性质和谱学分析鉴定了其中的 5个化合物 ,分别为 3 ,4 丙叉基苯甲酸 (2 ,2 dimethyl 1 ,3 dioxa benzo[d]pentane 6 carboxylicacid,Ⅰ )、水杨酸 (salicylicacid ,Ⅱ )、琥珀酸 (succinicacid ,Ⅲ )、胡萝卜苷 (daucosterol,Ⅳ )和己六醇 (1 ,2 ,3 ,4,5 ,6 hexanehexanol,Ⅴ )。结论化合物Ⅰ、Ⅱ、Ⅴ为首次从本属中分离得到的化合物     

芫花醋酸乙酯部位的化学成分研究

目的 研究芫花中醋酸乙酯部位化学成分.方法 分别采用聚酰胺柱色谱、硅胶柱色谱、Sephadex LH-20柱色谱等分离技术对芫花醋酸乙酯部位进行分离纯化,根据波谱数据和理化性质确定化合物的结构.结果 从芫花醋酸乙酯部位分离得到11个化合物,分别鉴定为松脂醇(1)、(一)-异落叶松脂素(2)、落叶松脂醇(3)、对羟基苯甲酸(4)、3,4-二羟基苯甲酸(5)、山柰酚-3-β-D-(6-O-反-p-香豆酰)葡萄糖苷(6)、山柰酚-3-β-D-(6-O-顺-p-香豆酰)葡萄糖苷(7)、芫花素(8)、3′-羟基芫花素(9)、芹菜素(10)、木犀草素(11).结论 化合物2、5、7为首次从该植物中分离得到.     

Three new lupane-type triterpenes from Ceriops tagal

Three new lupane-type triterpenes, 3α-O-trans-feruloylbetulinic acid (1), 3α-O-trans-coumaroylbetulinic acid (2) and 3β-O-cis-feruloylbetulin (3), together with 10 known triterpenes (4–13), were isolated from the aerial parts of the mangrove plant Ceriops tagal. The structures of the three new compounds were established by means of spectroscopic data analyses and chemical methods.     

反复早期自然流产患者绒毛、蜕膜组织中溶血磷脂酸受体3和环氧合酶2的表达

目的探讨反复早期自然流产患者绒毛、蜕膜组织中溶血磷脂酸受体3（lysophosphatidic acid receptor3,LPA3）和环氧合酶2（Cyclooxygenase2,COX2）的表达。方法采用免疫组化方法检测反复早期自然流产患者（研究组）30例以及同孕龄正常早孕女性（对照组）30例人工流产的绒毛、蜕膜组织中LP如和COX2的表达情况。结果研究组绒毛、蜕膜组织中LPA,和COX2的表达低于对照组,差异有统计学意义（P〈0．01）。结论绒毛、蜕膜组织中LP如及COX2表达降低可能导致反复早期自然流产的发生率增高。     

3-吡啶乙酸盐酸盐的合成

目的:合成3-吡啶乙酸盐酸盐.方法:以烟酸为起始原料,经酯化、缩合反应制得3-乙酰吡啶.3-乙酰吡啶经3-吡啶硫代乙酰吗啉,再水解、酸化得到3-吡啶乙酸盐酸盐.结果与结论:反应条件温和,原料价廉易得,适合工业化生产,以烟酸计,总收率达51.0%.     

超声波法合成3-肉桂酰异阿魏酸苯酯衍生物

异香(艹卓)醛和肉桂酸经酯化、与丙二酸在微波辐射下经Knoevenagel反应制得3-肉桂酰异阿魏酸后,再在超声波辐射下与取代酚酯化得到3-肉桂酰异阿魏酸苯酯,酯化收率为61%～84%.     

丙戊酸钠及其代谢产物与肝损伤的相关性分析

目的研究丙戊酸钠及3个代谢产物(2-丙基-4-五烯酸、3-羟基丙戊酸、5-羟基丙戊酸)对肝损伤参考指标的相关性分析。方法共收集328例癫痫患者血样,其中,123例肝功能异常癫痫患者血样为试验组,205例肝功能正常癫痫患者血样为对照组,采用LC-MS/MS方法测定两组血样(丙戊酸钠及代谢产物)的血药浓度,通过ROC曲线分析丙戊酸及其代谢产物浓度对肝功能异常的诊断价值。结果肝功能异常组患者丙戊酸钠及其3个代谢产物平均血药浓度均高于对照组,差异有统计学意义(P<0.05)。丙戊酸钠及其代谢产物的血药浓度均可作为诊断肝损伤的参考指标,5-羟基丙戊酸比丙戊酸钠有更好的诊断价值。结论丙戊酸钠代谢产物与肝毒性有关,能够作为肝损伤的诊断指标,可将其应用于临床,为丙戊酸钠有效给药提供参考。     

A new anti-HIV lupane acid from Gleditsia sinensis Lam.

A new lupane acid, 2β-carboxyl,3β-hydroxyl-norlupA (1)-20 (29)-en-28-oic acid (1), together with five known lupane acid derivatives (2-6), were isolated from the stings of Gleditsia sinensis Lam.. Their structures were elucidated on the basis of 1D and 2D NMR techniques. All these known compounds were isolated from this genus for the first time. The new compound 1 showed strong anti-HIV activity.     

含硫杀菌药叶枯灵代谢产物的合成

This paper reports the synthesis of the metabolites．1,3-dfthiolan-2-ylidenehydrazine(I)，acetic acid 1,3-dithiolan-2-ylidenehydrazide(II)，pyruvic acid 1,3-dithiolan-2-ylidenehydrazone(III)and benzoic acid l，3-dithiolan-2-ylidenehydrazide-S-oxide(IV)of yekuling，a new sulfurorganic fungicide(benzoic acid 1，3-dithiolan-2-ylidenehydrazide)．The structures of all the compounds synthesized were characterized by elemental analysis，IR，UV，MS and ¹HNMR spectra．     

Novel GHB-derived natural products from European mistletoe (Viscum album)

Abstract

Context: The European white-berry mistletoe [Viscum album L. (Loranthaceae)] is among the oldest known medicinal plants. At present the most important application of mistletoe extracts is in the treatment of cancer. However, natural products specific to mistletoe have rarely been encountered in the current literature.

Objective: To discover novel natural products specific to European mistletoe.

Materials and methods: European mistletoe was extracted with methanol, purified to partition against diethyl ether and further purified with XAD-7 column chromatography. Pure compounds were separated by Sephadex column chromatography and preparative HPLC. The structures of the novel compounds were established using a combination of several 2D NMR spectroscopic techniques and mass spectrometry.

Results: A new type of natural product derived from the methyl ester of γ-hydroxybutyric acid (GHB) coupled to hydroxybenzoic acids, namely 3-(3′-carbomethoxypropyl) gallic acid and 3-(3′-carbomethoxypropyl)-7→3″-protocatechoyl galloate were characterized from European white-berry mistletoe. Condensation of the 3-hydroxyl of gallic acid with the 4-hydroxyl of GHB significantly reduced the radical scavenging properties of the former compound.

Discussion and conclusion: The characterized compounds define a novel group of natural products that may be of particular interest because it appears that the two new compounds are not closely related to any known natural product.     

Immunotoxic effect of beta-chlorolactic acid on murine splenocyte and peritoneal macrophage function in vitro

β-Chlorolactic acid is a major intermediate of 3-monochloro-1,2-propanediol (MCPD) in mammalian species, which a well-known by-product of acid-hydrolyzed soy sauce during its manufacturing process. β-Chlorolactic acid has not been studied on immunotoxicity. To evaluate the immunomodulatory effect of β-chlorolactic acid on murine splenocyte and macrophage in vitro, we investigated splenocyte blastogenesis by concanavalin A (Con A), anti-CD3 and lipopolysaccharide (LPS), the production of cytokines from splenocyte, and the activity of mouse peritoneal macrophages. β-Chlorolactic acid suppressed significantly splenic blastogenesis to Con A or anti-CD3 from 8.5 to 54.7% at doses comprised between 200 and 800 μM. β-Chlorolactic acid also suppressed significantly splenic blastogeneis to LPS from 8.5 to 71.5% at doses comprised between 200 and 800 μM. The production level of interferon (IFN)-g on splenocyte culture with Con A was significantly reduced from 21.5 to 51.4% at the higher concentration than 100 μM of β-chlorolactic acid. The levels of interleukin (IL)-2 and IL-4 were also decreased 22.6–58.4 and 10.2–36.6%, respectively, at high concentrations of β-chlorolactic acid. There was a significant decrease from 6.1 to 40.8% in the production of nitric oxide (NO) by peritoneal macrophages treated with 400–1000 μM β-chlorolactic acid. These results indicate that β-chlorolactic acid might be able to induce immunotoxic effect on immune response of lymphocytes and peritoneal macrophages in vitro.     

卢帕他定中间体5-甲基吡啶-3-羧酸的合成工艺改进

目的:改进5-甲基吡啶-3-羧酸的合成工艺。方法:以3,5-二甲基吡啶为原料,经KMnO4氧化得卢帕他定中间体5-甲基吡啶-3-羧酸,经正交试验,优化工艺。结果:得出较佳的工艺条件,提高了产率,收率可达51％。结论:该方法易于工业化生产。