麦冬中甾体皂苷类化学成分研究

从麦冬70%乙醇提取物中,用Sp825大孔吸附树脂、ODS-C18等柱色谱分离得到6个甾体皂苷类成分。通过波谱分析及正反相色谱测定等手段全部鉴定出其结构,分别为麦冬皂苷D(1),麦冬皂苷D'(2),(25R)-Δ5(6)-烯-螺甾-3β,14α,17α-三羟基-3-O-α-L-吡喃鼠李糖基-(1→2)-β-D-吡喃葡萄糖苷(3),(25R)-龙血树皂苷F(4),(25R)-Δ5(6)-烯-螺甾-3β,14α-二羟基-3-O-α-L-吡喃鼠李糖基-(1→2)-[β-D-吡喃木糖基-(1→4)]-β-D-吡喃葡萄糖苷(5),偏诺皂苷元-3-O-α-L-吡喃鼠李糖基-(1→2)-[β-D-吡喃木糖基-(1→4)]-β-D-吡喃葡萄糖苷(6)。     

度他雄胺的合成分析

本文对前列腺增生治疗药物度他雄胺的合成进行分析,其初始原料我们采用的是孕烯酮酸(3-羰基-4-雄甾-烯17β-羧酸),为非那甾胺中间体,制备过程中主要的步骤为:3-羰基-4-雄甾-烯17β-羧酸C-4,5位氧化开环;成环;还原氢化形成3-氧代-4-氮杂-5α-雄甾-17β-羧酸;继续对C-20位酰基胺化得到(5α,17β)-N-[2,5-双(三氟甲基)苯基]-3-氧代-4-氮杂雄甾-17-甲酰胺;最后进行C-1,2位氧化脱氢制得度他雄胺,总收率为30.0%。本文对合成过程中各个中间过程进行分析,找出最适宜的反应条件,从而更好的节约原料成本,增加产率。     

海洋来源真菌Hypocrea virens菌丝体的化学成分研究

采用硅胶柱色谱、Sephadex LH-20凝胶柱色谱、开放ODS柱色谱以及HPLC等对海洋来源真菌Hypocreavirens的菌丝体进行化学成分分离,通过理化性质和波谱数据鉴定化合物的结构。从菌丝体的丙酮提取物中分离得到8个化合物,分别鉴定为1（10→6）Abeo-（22E,24R）-ergosta-5,7,9,22-tetraene-3α,11α-diol（Ⅰ）、24-甲烯基羊毛脂烷-8-烯-3β-醇（Ⅱ）、（22E,24R）-麦角甾-5,7,22-三烯-3β-醇（Ⅲ）、（22E,24R）-麦角甾-8,22-二烯-3β,5α,6β,7α-四醇（Ⅳ）、5α,9α-过氧-（22E,24R）-麦角甾-7,22-二烯-3β,6β-二醇（Ⅴ）、5α,8α-过氧-（22E,24R）-麦角甾-6,22-二烯-3β-醇（Ⅵ）、（22E,24R）-麦角甾-7,22-二烯-3β,5α,6β-三醇（Ⅶ）、3β,5α,9α-三羟基-（22E,24R）-麦角甾-7,22-二烯-6-酮（Ⅷ）,其中化合物Ⅰ、Ⅱ、Ⅳ、Ⅴ、Ⅷ均为首次从该属真菌中分离得到,化合物Ⅲ、Ⅵ、Ⅶ为首次从该种真菌中分离得到。     

银柴胡中α-菠甾醇和豆甾-7-烯醇含量测定的方法学研究

建立银柴胡中α-菠甾醇和豆甾-7-烯醇含量测定的方法。采用薄层扫描法,以525 nm为测定波长,700 nm为参比波长,α-菠甾醇(α-spinasterol)和豆甾-7-烯醇(stigmast-7-enol)的混合物(1:3)为对照品,测定银柴胡中α-菠甾醇和豆甾-7-烯醇的含量。α-菠甾醇和豆甾-7-烯醇含量在21.46~107.30μg/μL范围内呈良好的线性关系(r=0.991 1),平均回收率为99.5%(RSD=4.8%)。结论该方法简单、省时、损失小,可用于测定银柴胡中α-菠甾醇和豆甾-7-烯醇的含量。     

一种螺旋甾碱烷型糖苷生物碱及其制备方法与用途

正申请号:CN201710086724.6申请日:017.02.17公开(公告)号:CN106939031A本发明提供了一种螺旋甾碱烷型糖苷生物碱(3β,5α,22α,25R)螺旋甾碱烷-3-O-β-D-吡喃葡萄糖基-(1→2)-O-β-D-吡喃葡萄糖基-(1→4)-β-D-吡喃半乳糖苷及其制备方法与用途,该螺旋甾碱烷型糖苷生物碱对人肺腺癌细胞A549、人大细胞肺癌细胞H460和人肺鳞癌细胞SK-MES-1均具有抑制作用,且对A549细胞的半抑制     

蛋黄来源胆固醇中甾醇类杂质的研究

目的:研究胆固醇工艺中精制工序前后甾醇类杂质的变化,采用GC-MS方法对甾醇类杂质进行分析鉴定,同时获得符合欧洲药典标准的供注射用胆固醇。结论:从精制前胆固醇粗品中分析出10种甾醇类成分,分别是芥酸酰胺、胆固醇、24-脱氢胆固醇、5α-Cholest-8(14)-en-3-one、3β,4α,5α-4-methyl-8(14)-cholest-en-3-ol、3β-Ergosta-5,24-dien-3-ol、Δ5-菜油甾醇、4β-methyl-Cholesta-8,24-dien-3β-ol、α-环氧胆固醇、γ-谷甾醇。对制备出的胆固醇样品进行检测,产品质量符合欧洲药典要求。     

5α,8α-过氧化甾腙衍生物的合成及抗肿瘤活性评价

以脱氢表雄酮为原料,经多步反应合成5个侧链具有不同吲哚结构的过氧化甾腙衍生物。所有合成化合物都通过MS、1HNMR和13CNMR进行结构表征。另外,分别选用人肝癌细胞(Hep G2)、人乳腺癌细胞(MCF-7)和人正常肾上皮细胞(293T)对化合物的抗增殖活性进行评价,结果表明,3β-羟基-5α,8α-过氧化雄甾-6-烯-17-(5-氟-吲哚)腙和3β-羟基-5α,8α-过氧化雄甾-6-烯-17-(5-氯-吲哚)腙对所测试的肿瘤细胞株具有显著的抑制活性。     

新一代选择性醛固酮拮抗剂新药依普利酮的合成

合成新型甾体激素类化合物依普利酮(eplerenone)。以17β-羟基-3-氧代-11α-甲磺酸基-17α-孕甾-4-烯-7α,21-二羧酸,γ-内酯,7-甲酯(甲磺酸酯)为原料,经消除、环氧化反应得(7α,11α,17α)-9,11-环氧-17-羟基-3-氧代-孕甾-4-烯-7,21-二羧酸,γ-内酯,7-甲酯(依普利酮)。合成出依普利酮。经相关谱图(IR、1H-NMR)的表征,合成的化合物为目标化合物。     

刺齿贯众化学成分的研究

从鳞毛蕨科植物刺齿贯众(Cyrtomium caryotideum)地上部分通过溶剂提取、硅胶柱层析、SephadexLH-20柱层析和MCI柱层析等方法分离得到4个化合物,经核磁共振氢谱、碳谱和质谱确定了它们的结构,分别为山奈酚-3-O-β-D-葡萄糖苷(1)、山奈酚-3-O-β-D-芸香糖苷(2)、大黄素(3),5α,8α-过氧-(22E,24R)-麦角甾-6,22-二烯-3β-醇(4)。化合物3和4为首次从本植物中分离得到。     

两个多羟基甾醇的分离与结构鉴定

研究刺柳珊瑚Echinogorgia sp的化学成分。各种色谱方法进行分离纯化,理化性质和光谱数据鉴定结构。从中国南海硇洲岛刺柳珊瑚Echinogorgia sp中分离得到两个多羟基甾醇：胆甾-3β,5α,6β,11β-四醇;胆甾-22（23）-烯-3β,5α,6β,11β-四醇,这些化合物均为首次从该属珊瑚中获得。     

Insect antifeedant properties of anthranoids from the genusVismia

Vismiones and ferruginins, representatives of a new class of lypophilic anthranoids from the genusVismia were found to inhibit feeding in larvae of species ofSpodoptera, Heliothis, and inLocusta migratoria.     

Direct observation of freeze-thaw instability of latex coatings via high pressure freezing and cryogenic SEM

Despite its industrial importance, the subject of freeze-thaw (F/T) stability of latex coatings has not been studied extensively. There is also a lack of fundamental understanding about the process and the mechanisms through which a coating becomes destabilized. High pressure (2100 bar) freezing fixes the state of water-suspended particles of polymer binder and inorganic pigments without the growth of ice crystals during freezing that produce artifacts in direct imaging scanning electron microscopy (SEM) of fracture surfaces of frozen coatings. We show that by incorporating copolymerizable functional monomers, it is possible to achieve F/T stability in polymer latexes and in low-VOC paints, as judged by the microstructures revealed by the cryogenic SEM technique. Particle coalescence as well as pigment segregation in F/T unstable systems are visualized. In order to achieve F/T stability in paints, latex particles must not flocculate and should provide protection to inorganic pigment and extender particles. Because of the unique capabilities of the cryogenic SEM, we are able to separate the effects of freezing and thawing, and study the influence of the rate of freezing and thawing on F/T stability. Destabilization can be caused by either freezing or thawing. A slow freezing process is more detrimental to F/T stability than a fast freezing process; the latter actually preserves suspension stability during freezing. Presented at the 82nd Annual Meeting of the Federation of Societies for Coatings Technology, October 27–29, 2004 in Chicago, IL. Tied for first place in The John A. Gordon Best Paper Competition.     

Ethanol and (−)-α-Pinene: Attractant Kairomones for Bark and Ambrosia Beetles in the Southeastern US

In 2002–2004, we examined the flight responses of 49 species of native and exotic bark and ambrosia beetles (Coleoptera: Scolytidae and Platypodidae) to traps baited with ethanol and/or (−)-α-pinene in the southeastern US. Eight field trials were conducted in mature pine stands in Alabama, Florida, Georgia, North Carolina, and South Carolina. Funnel traps baited with ethanol lures (release rate, about 0.6 g/day at 25–28°C) were attractive to ten species of ambrosia beetles (Ambrosiodmus tachygraphus, Anisandrus sayi, Dryoxylon onoharaensum, Monarthrum mali, Xyleborinus saxesenii, Xyleborus affinis, Xyleborus ferrugineus, Xylosandrus compactus, Xylosandrus crassiusculus, and Xylosandrus germanus) and two species of bark beetles (Cryptocarenus heveae and Hypothenemus sp.). Traps baited with (−)-α-pinene lures (release rate, 2–6 g/day at 25–28°C) were attractive to five bark beetle species (Dendroctonus terebrans, Hylastes porculus, Hylastes salebrosus, Hylastes tenuis, and Ips grandicollis) and one platypodid ambrosia beetle species (Myoplatypus flavicornis). Ethanol enhanced responses of some species (Xyleborus pubescens, H. porculus, H. salebrosus, H. tenuis, and Pityophthorus cariniceps) to traps baited with (−)-α-pinene in some locations. (−)-α-Pinene interrupted the response of some ambrosia beetle species to traps baited with ethanol, but only the response of D. onoharaensum was interrupted consistently at most locations. Of 23 species of ambrosia beetles captured in our field trials, nine were exotic and accounted for 70–97% of total catches of ambrosia beetles. Our results provide support for the continued use of separate traps baited with ethanol alone and ethanol with (−)-α-pinene to detect and monitor common bark and ambrosia beetles from the southeastern region of the US.     

Methyl 2,4,6-decatrienoates Attract Stink Bugs and Tachinid Parasitoids

Halyomorpha halys (Stål) (Pentatomidae), called the brown marmorated stink bug (BMSB), is a newly invasive species in the eastern USA that is rapidly spreading from the original point of establishment in Allentown, PA. In its native range, the BMSB is reportedly attracted to methyl (E,E,Z)-2,4,6-decatrienoate, the male-produced pheromone of another pentatomid common in eastern Asia, Plautia stali Scott. In North America, Thyanta spp. are the only pentatomids known to produce methyl 2,4,6-decatrienoate [the (E,Z,Z)-isomer] as part of their pheromones. Methyl 2,4,6-decatrienoates were field-tested in Maryland to monitor the spread of the BMSB and to explore the possibility that Thyanta spp. are an alternate host for parasitic tachinid flies that use stink bug pheromones as host-finding kairomones. Here we report the first captures of adult and nymph BMSBs in traps baited with methyl (E,E,Z)-2,4,6-decatrienoate in central Maryland and present data verifying that the tachinid, Euclytia flava (Townsend), exploits methyl (E,Z,Z)-2,4,6-decatrienoate as a kairomone. We also report the unexpected finding that various isomers of methyl 2,4,6-decatrienoate attract Acrosternum hilare (Say), although this bug apparently does not produce methyl decatrienoates. Other stink bugs and tachinids native to North America were also attracted to methyl 2,4,6-decatrienoates. These data indicate there are Heteroptera in North America in addition to Thyanta spp. that probably use methyl 2,4,6-decatrienoates as pheromones. The evidence that some pentatomids exploit the pheromones of other true bugs as kairomones to find food or to congregate as a passive defense against tachinid parasitism is discussed.     

2007～2008年世界塑料工业进展

收集了2007年7月～2008年6月世界塑料工业的相关资料,介绍了2007～2008年国外塑料工业的发展情况,提供了世界塑料产量、消费量及全球各类树脂的需求量及产能情况.按通用热塑性树脂(聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂)、工程塑料(尼龙、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚)、特种工程塑料(聚苯·硫醚、液晶聚合物、聚醚醚酮)、通用热固性树脂(酚醛、聚氨酯、不饱和聚酯树脂、环氧树脂)不同品种的顺序,对树脂的产量、消费量、供需状况及合成工艺、产品应用开发、树脂品种的延伸及应用的进一步扩展等技术作了详细介绍.     

2005～2006年国外塑料工业进展

收集了2005年7月～2006年6月国外塑料工业的相关资料,介绍了2005—2006年国外塑料工业的发展情况。提供了世界塑料产量、消费量及全球各类树脂生产量以及各国塑料制品的进出口情况。作为对比,介绍了中国塑料的生产情况。按通用热塑性树脂（聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、ABS树脂）、工程塑料（聚酰胺、聚碳酸酯、聚甲醛、热塑性聚酯、聚苯醚）、通用热固性树脂（酚醛、聚氨酯、不饱和树脂、环氧树脂）、特种工程塑料（聚苯硫醚、液晶聚合物、聚醚醚酮）的品种顺序,对树脂的产量、消费量、供需状况及合成工艺、产品开发、树脂品种的延伸及应用的扩展作了详细的介绍。