左氧氟沙星制备方法的改进研究

目的:改进左氧氟沙星的制备工艺。方法:用DMF作溶剂,以三乙胺为催化剂,左氧氟羧酸与N-甲基哌嗪缩合制备左氧氟沙星。结果:制得左氧氟沙星的纯度稳定在99%以上,且目标产物经核磁共振、IR及MS确认结构。结论:本工艺改进了反应条件,减少了环境污染,降低了成本,具有更高的经济效益和市场竞争力。     

左氧氟沙星合成工艺改进研究

对左氧氟沙星的工艺进行了优化,以(2,3,4,5)-四氟苯甲酰氯为起始原料,经酰化,胺化,环合制得左氧氟环合酯,然后用无水哌嗪与左氧氟环合酯缩合,经硫酸二甲酯甲基化后水解精制得左氧氟沙星。与原工艺相比,用无水哌嗪代替N-甲基哌嗪,提高了产品的收率和质量,降低了成本,减少了环境污染,技术指标符合CP2010左氧氟沙星要求。     

旋光-紫外分析法测定盐酸左氧氟沙星滴眼液中左氧氟沙星的含量

选择旋光分析法测定盐酸左氧氟沙星滴眼液中左氧氟沙星的含量,利用紫外-可见分光光度法测定其氧氟沙星的总量,从而建立起氧氟沙星左旋体含量测定的新方法,打破氧氟沙星左旋体含量的传统测量方法-高效液相色谱法,为该类滴眼液的质量标准和控制方法提供了实验依据。左氧氟沙星在1～10 mg/mL范围内线性关系良好（r=0.9867,n=6）,加样回收率在120%左右,结果表明,盐酸左氧氟沙星滴眼液中左氧氟沙星的含量范围为100.9%～103.9%。该方法灵敏、准确、重现性好,结果令人满意。     

树状大分子与乳酸左氧氟沙星的相互作用研究

通过发散法合成出1.0~3.0 G聚酰胺—胺型树枝状高分子(PAMAM),利用氨基与醛的脱水缩合反应,用水杨醛修饰树状高分子合成出PAMAM-水杨醛席夫碱(PAMAM-SA),并采用荧光光谱法以中性磷酸盐缓冲溶液为介质,研究不同代数PAMAM及PAMAM-SA与乳酸左氧氟沙星的相互作用。结果表明:不同代数的PAMAM-SA都能引起乳酸左氧氟沙星(LFL)荧光强度降低,且PAMAM-SA对乳酸左氧氟沙星的猝灭属静态猝灭。与修饰前的PAMAM比较,经水杨醛修饰的PAMAM的树状大分子与乳酸左氧氟沙星的相互作用均表现出较强的相互作用。     

稳定同位素标记物D_3-左氧氟沙星的合成及表征

以市售的左氧氟沙星羧酸为原料,以氘代甲醇为稳定同位素标记物前体,经无水哌嗪取代、双氘代甲基化、氢氧化钠水解合成出稳定同位素标记的D_3-左氧氟沙星,3步反应总收率为45.5%。目标产物经MS、~1HNMR表征确认,通过高效液相色谱确认化学纯度98%,经计算同位素丰度为97.7%。该合成路线具有操作简便、试剂廉价等优点。     

甲磺酸帕珠沙星的合成

以左氧氟沙星中间体(S)-9,10-二氟-3-甲基-7-氧代-2,3-二氢-7-H吡啶[1,2,3-de][1,4]苯并噁嗪-6-羧酸乙酯为起始原料,经与氰乙酸乙酯进行亲核取代反应、水解脱羧、环合、水解、Hoffman降解,与甲磺酸成盐得甲磺酸帕珠沙星,总收率为38%,产品纯度符合药用标准。     

甲磺酸帕珠沙星的合成工艺改进

以左氧氟沙星的中间体--(S)-9,10-二氟-3-甲基-7-氧代-2,3-二氢-7H-吡啶[1,2,3-de][1,4]苯并噁嗪-6-羧酸乙酯为起始原料,经过与氰乙酸乙酯缩合、水解脱羧、1,2-二溴乙烷环合、水解、霍夫曼降解、成盐得到喹诺酮类抗菌药甲磺酸帕珠沙星.总收率达到43.8%,并对目标产物,进行了元素分析,IR,1H NMR,13C NMR,MS等确认.与文献报道相比,该合成工艺路线具有反应条件温和,收率较高,适合工业化生产.     

"一锅法"合成左氧氟沙星

以左氧氟环合酯为原料,水解后直接与N-甲基哌嗪缩合反应,"一锅法"合成左氧氟沙星.该合成方法产品收率高、三废少、生产效率高,符合绿色化学理念.     

金属改性MCM-41对盐酸左氧氟沙星吸附研究

实验制备MCM-41及金属改性Al-MCM-41和Co-MCM-41,并作为吸附剂来处理废水中的盐酸左氧氟沙星.实验对吸附剂反应温度、pH、吸附剂投加量对废水中盐酸左氧氟沙星的吸附效率的影响进行了研究.根据实验结果,设计一款有效吸附废水中的盐酸左氧氟沙星吸附装置,该装置有望于应用于实际生产中,从而简化处理抗生素盐酸左氧...     

磁性分子印迹技术在药物分析学创新实验中的应用

为拓展药学专业大学生创新思维水平、规范实验操作以及提高分析实验数据能力,在大学生创新创业项目执行中采用PBL教学方法,加强综合素质。本实验以左氧氟沙星为模板分子,衣康酸为功能单体,乙二醇二甲基丙烯酸酯为交联剂,2,2-偶氮二异丁腈为引发剂,制备左氧氟沙星磁性表面分子印迹聚合物,通过透射电子显微镜、红外光谱等对材料进行表征,并对婴幼儿配方奶粉中左氧氟沙星开展选择性分离富集。     

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.     

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。     

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.