反相高效液相色谱法测定3种中成药中的葛根素

 建立了测定小儿清感灵片、步长新脑心通胶囊和感冒清热颗粒 3种中成药中葛根素含量的反相高效液相色谱方法。采用APEXODS色谱柱 ,以醋酸铵缓冲液 (10 0mmol/L ,pH 5 0 ) 甲醇 (体积比为 75∶2 5 )的混合溶液为流动相 ,检测波长为 2 5 0nm ,流速为 0 8mL/min。葛根素在 2mg/L～ 2 0mg/L时其色谱峰面积与质量浓度的线性关系良好 (r =0 9999) ;上述 3种中成药中的葛根素含量分别为 3 48mg/g ,1 0 8mg/ g及 1 5 2mg/ g(蔗糖型 ) ;其加样回收率分别为 99 0 % ,93 4%和 97 5 %。该法简便、快速、专属性强 ,可以作为多种中药制剂中葛根素含量的测定方法。     

四磺化酞菁钴在微乳液、醇-水体系中的二聚现象研究

采用分光光度法研究了四磺化酞菁钴（ＣｏＴＳＰｃ），在微乳液（ＴｒｉｔｏｎＸ－１００－壬烷－正戊醇－水）、醇－水（甲醇、乙醇、丙醇）体系中的二聚现象，计算了ＣｏＴＳＰｃ的二聚常数ＫＤ。结果表明，ＣｏＴＳＰｃ的二聚常数ＫＤ值随着微乳液中表面活性的浓度及醇－水溶液的介电常数的增加而减小。     

羧甲基纤维素系列高分子表面活性剂超声合成的研究

研究了在超声波作用下羧甲基纤维素的降解反应及ＣＭＣ与具有不同亲水亲油比值的活性大单体「烷基醇（酚）聚氧乙烯醚丙烯酸酯及第三单体」的超声共聚反应。经萃取提纯的共聚产物用ＩＲ，＾１３Ｃ ＮＭＲ和ＵＶ等方法进行表证，证实通过超声反应制得了二元和三元共聚物。     

STUDIES ON THE MECHANISM OF VINYL PHOTOPOLYMERIZATION INITIATED BY CONDENSED AROMATIC HYDROCARBON-ANILINE SYSTEMS

Initiation mechanism of the photopolymerization of acrylonitrile and methyl methacrylate, usingbinary condensed aromatic hydrocarbon (CAH)-aniline systems as initiator, was studied. The strongerthe electron-donating ability of the aniline derivatives, the faster the the of photopolymerizationwill be. The radical intermediates produced by photoreaction between anthracene and anilinewere detected with ESR spectra. The initiation scheme involves the formation of exciplex betweenthe excited singlet state of CAH and the ground state of aniline as the first step, and then followedby proton transfer, leading to the generation of two kinds of radicals. From the end-group analysisof the polymers obtained, it is suggested that both kinds of radicals are involved in the initiation.     

纳米氧化铝负载双硫腙分离富集-原子吸收法测定地质样品中的金、铂、钯的研究

金、铂、钯在地质样品中的含量甚微,国内外常采用ICP-AES,ICP-MS和ETAAS直接测定。FAAS法由于仪器便宜、操作方便,也广泛应用于预富集后的痕量贵金属的分析。目前,在测定贵金属的分析方法中,常采用固相萃取法富集分离样品,主要的固相萃取剂有:无机吸附剂,交联树脂[1],螯合树脂[     

Synthesis and Crystal Structure of a New Organic-inorganic Hybrid One-dimensional Polymer： [Zn（C8H23N5）]2（Pb3I10）

1 INTRODUCTION Recently, the organic-inorganic hybrid Ⅳa groupmetal halides with low-dimensional structure haveattracted much attention of chemists and physicistsdue to their particular properties and applications.For example, they are akin to “natural quantum-well”architectures and have tunable excitonic propertiesusually governed by the inorganic substructure andorganic component[1]; they have been applied assome technologically important materials, such assemiconductor materials in …     

Crystal Structures and Magnetic Studies of Naphthalene Derivatives Containing Nitronly Nitroxides

Crystal structures of new nitronyl nitroxide derivatives 1, 2 and 3 were determined with X‐ray diffraction analysis: 1, monoclinic, C₂/c, a = 1.2404(5) nm, b = 0.9730(5) um, c = 2.7049(10) ran, β = 98.189(15)°, V = 3.2315(24) nm³, Z = 8; 2, or‐thorhombic, Pbca, a = 0.61262(2) nm, b = 1.11426(6) nm, c = 2.30543(13) nm, V = 1.57373(13) nm³, Z = 4; 3, monoclinic, P2(1)/n, a=0.64253(4) nm, b=2.55003(17) nm, c = 1.15497(6) nm, β = 95.000(3)°, V = 1.8852(2) nm³, Z = 4. Their magnetic properties were measured with SQUID and analyzed based on their crystal structures with simple singlet‐triplet, modified one dimensional antiferromagnetic chain and modified singlet‐triplet models respectively: 1, J/k_b= ?2.5 K; 2, J/k_b = 7.8 K, θ = 2.8 K; 3, J/k_b = ?0.96 K, θ = 0.21 K.     

对固体圆二色光谱测试方法的再认识——兼谈“浓度效应”

对近期发展的固体圆二色(CD)光谱测试方法进行了概述、评价和比较, 着重探讨了“浓度效应”的存在使固体CD光谱失真的原因. 通过对本课题组和其他作者已报道的四种化合物的固体CD谱再测试的反思, 强调了依手性化合物的手性光谱学性质不同, 根据浓度梯度实验选择其合适测试浓度的必要性. 对固有手性的阻转异构化合物(S)-1,1'-联二萘酚(S-BINOL)进行了成膜法固体CD谱浓度梯度测试, 发现所得固体薄膜CD谱中也存在着“浓度效应”     

有机/无机杂化材料担载季铵盐催化剂的制备及其在相转移催化反应中的应用

利用溶胶-凝胶(S0l-gel)技术制备了新型的有机／无机杂化材料担载的季铵盐催化剂。优化了制备方法、反应条件等多种因素；考察了其作为相转移催化剂在1-溴代正庚烷与碘化钾的亲核取代反应中的应用，转化率最高可达到95％。     

自制苯乙烯-丙烯酸乙酯共聚物与PEG20M复合萃取涂层用于洗涤制品中1,4-氧杂环己烷的测定

采用顶空固相微萃取-毛细管气相色谱联用技术测定了洗涤制品中的1,4-二氧杂环己烷.使用自制的萃取头(苯乙烯-丙烯酸乙酯共聚物与PEG20M复合)于顶空平衡温度80℃下萃取样品40 min.萃取物用内壁涂有SE-30固定液的石英毛细管柱分离,外标法定量.1,4-二氧杂环己烷含量为0.35～120 μg/g时,其峰面积与含量呈良好的线性关系(r=0.999 8);回收率为98.7%～102%;相对标准偏差(n=5)为9.33%.