左旋麻黄素半生物合成研究Ⅲ.L-苯基乙酰基甲醇的提取技术

对固相生物合成的L PAC(左旋麻黄素前体 )提取技术进行了研究。结果表明 ,采用H型大孔吸附树脂从生物合成的反应产物中提取L PAC最佳。当样品液pH为 6左右、过柱流速为0 2～ 0 3BV/min、柱直径与树脂高度比为 1 5∶11,用质量分数为 70 %丙酮水溶液洗脱 ,该大孔吸附树脂对L PAC的动态吸附量为 6 1 6 9mg/g。洗脱的丙酮水溶液经减压浓缩 ,获油状L PAC粗品 ,其质量浓度不低于 0 2 4g/mL     

延龄草苷的制备

延龄草苷是中药中的一个有效成分,采用提取分离的方法从中药材大量获得它是困难的.我们以易得的原料薯蓣皂素和葡萄糖为原料合成了它.首先从葡萄糖起始,通过酰化、溴代反应,采用一锅煮的方法合成中间体溴-D-四乙酰葡萄糖;再与薯蓣皂素通过催化剂Hg(Ac)催化立体选择性的生成β-苷键,水解反应制备得到延龄草苷,总产率38.2%。反应条件温和,适于大量制备。产物结构通过IR,1HNMR和MS确证。     

吸毒现场吸毒工具中的甲基苯丙胺分析

Based on the details in the case, the analysis method of methamphetamine was built up, which is supposed to be used for in vitro material taken from the criminal scene. It is suggested that GC-FID is first used for methamphetamine concentration scanning. Thus, according to the results, the sample could be concentrated or diluted for the next GC/MS analysis. Using this procedure, the satisfying result was achieved.     

Methamphetamine impairs sexual motivation but not sexual performance in male Japanese quail.

The present study investigated the effects of chronic pre-exposure to methamphetamine on sexual motivation and performance in male Japanese quail. Quail were pre-exposed to methamphetamine (1.0 or 3.0 mg/kg ip) or saline (ip) once daily for 10 days and locomotor activity was measured. After a 10 day washout period, sexual motivation was measured in a straight-arm runway with visual access to a female at one end. Three to 5 hr after sexual motivation tests, males were allowed to copulate with a receptive female quail and copulatory behavior was assessed. Tests were conducted once per day for 10 days. Results showed that males pre-exposed to methamphetamine had decreased locomotor activity compared to saline controls. Males pre-exposed to METH later ran slower toward a female in the runway and spent less time near her. In contrast, methamphetamine pre-exposed males showed similar copulatory behavior as saline pre-exposed males. The findings suggest that chronic pre-exposure to methamphetamine may impair sexual motivation but not sexual performance. The findings are discussed from a comparative perspective and with regard to their clinical relevance. (PsycINFO Database Record (c) 2010 APA, all rights reserved)     

乙酰－L－肉毒碱的合成

研究了用ｌ－肉毒碱和乙酰氯为原料，以对甲苯磺酸为催化剂，冰乙酸为溶剂合成乙酰－ｌ－肉毒碱的方法，得出最佳反应温度为７０℃，最佳物料配比为：ｌ－肉毒碱：乙酰氯：对甲苯磺股＝１：９：０．３（摩尔比），反应收率达７８．１％，改进了提纯乙酰－ｌ－肉毒碱的方法．     

“摇头丸”片剂的GC／MS检验

对一例缉获的"摇头丸"片剂毒品进行了GC/MS快速定性、定量检验,检出主要毒品成份为甲基苯丙胺,添加剂有麻黄素、咖啡因、氯胺酮,并对其含量和合成情况进行了分析.工作曲线为C(mg/L)=3.281 7×10-6×A+0.015 92,相关系数r=0.997 2;平均回收率90.3%,标准偏差0.65,变异系数1.3%(n=5);样品含量为7.35%.为分析、推断该类毒品的制作过程提供了一定的借鉴作用.     

乙酰氯法测定含环氧基聚酯羟值

介绍了一种含环氧基聚酯的羟值测定方法,即乙酰氯法。通过对其酰化原理分析,选用乙酰氯作酰化剂、二氯甲烷作酰化溶剂,测定含环氧基聚酯的羟值。结果发现无抱团现象,测定结果误差较小。     

全基团保护法制备三氯蔗糖的研究

全基团保护法包括蔗糖 8个羟基团的完全保护、蔗糖 3个伯羟基的去保护作用、4 C位乙酰基向 6 C的迁移、对特定游离羟基团的氯化与脱除剩余保护基团等 5个步骤。其中 ,若采用碱性乙酰基迁移法 ,则乙酰基迁移与氯化反应 2步可合并为 1步。通过大量的试验 ,确定了具体的制备路线与各反应步骤之间的适宜组合方案 ,优化各种工艺参数 ,使三氯蔗糖终产品的得率达到 2 8 1 %。     

高纯乙酰氯生产工艺的改进

通过对国内乙酰氯现有生产工艺的考察、研究,对传统的醋酸和三氯化磷合成法进行了工艺改进,改进后工艺的产品收率比原来提高近6%,达到96.3%以上,产品质量达到99.0%以上,反应条件更加温和,操作容易控制,基本无三废产生,生产成本明显降低。     

RGS4和D2受体信号通路相关分子在甲基苯丙胺依赖CPP大鼠纹状体的表达变化

目的:研究甲基苯丙胺(methamphetamine, METH)依赖条件性位置偏爱(conditioned place preference, CPP) 实验大鼠纹状体G蛋白信号调节因子4(regulator of G-protein signal 4,RGS4)和多巴胺D2受体(dopamine receptor D2)信号通路相关分子的表达变化。方法: 建立METH依赖CPP大鼠 1周组、2周组,应用蛋白质印迹(Western blot)测定各组大鼠纹状体RGS4和D2、抑制性G蛋白α亚基(inhibitory G protein α-subunit,Gαi)、丝裂原激活的蛋白激酶(mitogen-activated protein kinase,MAPK)蛋白表达的变化;应用酶联免疫吸附试验(enzyme linked immunosorbent assay,ELISA)测定各组大鼠纹状体环磷酸腺苷(cyclic adenosine monophosphate,cAMP)含量的变化。结果: 与生理盐水对照组相比,METH依赖1周组、2周组大鼠在伴药箱的平均停留时间明显延长(P<0.05)。与生理盐水对照组相比,RGS4蛋白在METH依赖1周、2周组的表达均明显下降(P<0.01),且与METH依赖1周组相比,2周组的下降更为明显(P<0.05);与生理盐水对照组相比, D2、Gαi、MAPK蛋白以及cAMP在METH依赖1周、2周组的表达均明显升高(P<0.01),且与METH依赖1周组相比,2周组的升高更为明显(P<0.05)。结论:在METH依赖的CPP大鼠纹状体中,RGS4和D2受体信号传导通路相关分子发生了改变,RGS4可能参与了METH依赖的CPP大鼠纹状体D2受体信号传导通路的调节。