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1.
Triterpenoid Constituents of Huperzia miyoshiana 总被引:1,自引:0,他引:1
Thirteen triterpenoids, including three new ones, miyoshianois A (1), B (2) and C (3), were isolated from Huperzia miyoshiana. The structures of these new compounds were established as 3-O-dihydroferuloyltohogenol (1), 16-oxo-3β,21β-dihydrox-y-serrat-14-en-24-ferulate (2) and 16-oxo-3a, 21β-dihydroxy-serrat-14-en-24-ferulate (3), respectively, on the basis of their spectroscopic analysis. 相似文献
2.
α-巯基乙胺盐酸盐的合成 总被引:2,自引:0,他引:2
α-巯基乙胺盐酸盐的合成周慧,黄静(中国科学院成都有机化学研究所成都,610015)(华西医科大学药学院成都,610044)关键词巯基乙胺,合成前言α-巯基乙胺不仅是重要的化工原料,而且是许多抗溃疡药物如甲氰咪胍、雷尼替丁等的重要中间体 ̄[1],同时... 相似文献
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制备了ITO/Gr/CH_3NH_3PbI_3/CS/GOx电极,将制得的电极浸入5.0mL的0.1mol·L~(-1) PBS(pH 7.0)中,加入丁草胺标准溶液,保持10min,然后将电极取出插入含有0.8mmol·L~(-1)葡萄糖的0.1mol·L~(-1) PBS(pH 7.0)中,测量光电流(I)。另做空白试验(操作同上,但不存在丁草胺),测量光电流(I_0)。由(I_0-I)/I_0×100计算丁草胺对光电流的抑制率。结果表明,抑制率与丁草胺的浓度在0.02~10.0nmol·L~(-1)内呈线性关系,检出限(3S/N)为0.005nmol·L~(-1)。方法用于测定蔬菜和水果空白加标样品中的丁草胺,测定值与气相色谱-质谱法的测定结果一致,测定值的相对标准偏差(n=6)在1.8%~4.7%之间,加标回收率在93.3%~102%之间。 相似文献
4.
Owing to no complications caused by solid supports, such as adsorptive sample loss and deactivation, tailing of solute peaks, and contamination, countercurrent chromatography (CCC) has been an area of intense research since the first introduction of CCC in 1970,[1] and various apparatus and broad applications have been advanced[2,3]. For these developments, the type-J synchronous planet centrifuge has received considerable attention, which relies not only on its relatively simple mechanic design, but also on its high partition efficiency and short elution time caused by mixing and settling for the efficient chromatographic separations. In the past, however, almost all of type-J centrifuges rotated slowly were disposed horizontally due to the original design and some experiments that gravis plays an important role at a low rotary speed as similar to type-V rotating multilayer helical tube in unit gravity[4-9]. In fact,we discovered that the upright apparatus holds more retention of stationary phase than the horiziontal aparatus when large standard tubings were used as mutilayer coil column and the aparatus was operated under same contions. We report here a new coil planet centrifuge with four upright cylindrical columns for large scale countercurrent chromatographic preparation. The design principle and apparatus of UCCC is as samilar to type-J multilayer coil planet centrifuge. Four uptight cylindrical column holders are symmetrically arranged around the centrifuge axis as similar to the type-J HSCCC with three horizontal multilayer coils connected in series[8] . A series of experiments indicat that upright CCC has many advantages over the horizontal CCC when using a large-bore tube as multilayer coil column for large scale countercurrent chromatographic separation.Upright CCC provide a versatile countercurrent chromatographic method for large-scale preparation from very crude sample. It has good preparative capacity and flexible suitability to various sample and two-phase system.The present apparatus not only can be operated at a high speed as similar as commonly used HSCCC for the system having short settling time and but also can be run at a low speed for the system having relative long settling time. Because of automatical control and seal-free flow through device, the uptight CCC apparatus may be readily scaled up to industrial preparation. 相似文献
5.
2-巯基-5-甲基-1,3,4-噻二唑(2-mercapto-5-Methyl-1,3,4-thiadiazole,以下简称噻二唑)是一种用途广泛的有机杂环化合物,也是合成先锋霉素5号[1](cefazolin)的中间体之一.此外研究发现,含有1,3,4-噻二唑的衍生物具有除草、植物生长调节,杀菌,消炎,抗癌,降压,及降低胆固酵等多种生物、生理活性[2,3].因此,噻二唑的合成研究一直为人们所关注[4],而在合成工艺的优化过程中,质谱可发挥监控反应的重要作用. 相似文献
6.
采用体外酶抑制活性检测方法结合超滤质谱(UF-LC/MS)筛选方法对中药提取物中的α-葡萄糖苷酶抑制剂进行了筛选.以4-硝基苯-α-D-吡喃葡萄糖苷(PNPG)为底物,阿卡波糖为阳性对照药,对5种富含黄酮类化合物的中药提取物进行了α-葡萄糖苷酶抑制活性的初步测定.结果表明,银杏叶具有最强的α-葡萄糖苷酶抑制活性,可作为进一步复筛的对象.利用超滤质谱技术对银杏叶中潜在的α-葡萄糖苷酶抑制剂进行了筛选,从中筛选出4种潜在的α-葡萄糖苷酶抑制剂,并利用液相色谱-串联质谱技术(LC-MSn)对其结构进行了鉴定.本文结果为开发新一代安全有效的降糖药物奠定了基础. 相似文献
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