硫普罗宁的药代动力学及光度法测定

建立了光度法测定硫普罗宁的新方法。研究表明:在SCN-和KNO3存在下,控制溶液pH4.0,Cu(II)被硫普罗宁还原生成的Cu(I)与SCN-反应形成CuSCN沉淀,该沉淀能浮在水相表面。通过测定溶液中剩余Cu(II)的量,可以测定硫普罗宁的含量。吸光度与硫普罗宁浓度之间存在良好线性关系。线性方程:A=4.898-0.3616ρ(μg/mL),线性范围为0.25～12.0μg/mL,相关系数R=0.9993,检出限为0.16μg/mL。该方法可直接用于药物中硫普罗宁含量的测定及其药代动力学行为研究。     

Indirect determination of cefradine with n-propyl alcohol-ammonium sulfate-water system by extraction-flotation of cuprous thiocyanate

A new method was developed for the determination of cefradine by extraction-flotation of CuSCN.The experiment indicated that in the presence of 0.20 mol/L NaOH the degradation of cefradine took place in water bath at 100℃.The thiol group(-SH)of the degradation product could reduce Cu(Ⅱ)to Cu(Ⅰ)for the formation of the emulsion CuSCN in the presence of NH_4SCN at pH 4.0.By determining the residual amount of Cu(Ⅱ)in the solution and calculating the flotation yield of Cu(Ⅱ),the indirect determination of cefradine can be obtained.This method has been applied to determine cefradine in capsules,human serum and urine samples,respectively.     

活性炭吸附及离子交换富集分离-分光光度法测定水中痕量银

建立了用活性炭对水中痕量银进行预富集的新方法。结果表明,pH=1.0时,活性炭能对水中被抗坏血酸还原后的痕量银进行吸附富集,而Cu(Ⅱ)、Fe(Ⅲ)、Co(Ⅱ)、Ni(Ⅱ)、Pb(Ⅱ)、Zn(Ⅱ)、Mn(Ⅱ)、Al(Ⅲ)、Bi(Ⅲ)和Sb(Ⅲ)等常见阳离子不被吸附,用K2S2O8将吸附在活性炭上的单质银氧化解脱后,用Mg(NO3)2辅助置换洗脱,可用分光光度法测定。该法在8～50μg/L银(Ⅰ)范围内加标回收率为93.2～97.1%。同时还研究了活性炭对银的吸附行为,提出了活性炭表面上被氧化的Ag(Ⅰ)和Mg(Ⅱ)有离子交换作用。应用该法测定自来水中痕量银,结果令人满意。     

在NaCl和SCN~-存在下浮选铜(Ⅱ)间接测定十六烷基三甲基溴化铵

研究了NaCl和NH4SCN浮选Cu(Ⅱ)间接测定十六烷基三甲基溴化铵的新方法。在水溶液中,Cu(Ⅱ)与SCN-和CTMAB缔合生成沉淀,在NaCl存在下,此沉淀被浮选。实验表明,Cu(Ⅱ)的浮选率与CTMAB的量在3.6~54.7 mg/L范围内呈良好的线性关系。CTMAB的检出限为1.8μg/mL。方法已用于合成水样和自来水中CTMAB的测定。     

A New Dinuclear Cu(Ⅱ) Complex of a Ligand with Benzimidazole Group - Synthesis and Crystal Structure

A new dinuclear copper complex, [Cu(C9H11N3)Cl2]2(C18H22Cl4Cu2N6), has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic P-1 space group with a = 7.526(3), b = 9.473(4), c = 9.535(3)(A), α = 117.214(10), β = 108.251(9), γ = 91.560(6)°, V = 562.3(4)(A)3, Z = 1, Mr = 591.30, F(000) = 298, Dc = 1.746 g/cm3, μ(MoKα) = 2.385 mm-1, the final R = 0.0577 and wR = 0.1248 for 2188 unique reflections with 1629 observed ones (Ⅰ＞ 2σ(Ⅰ)). In the title complex, each copper(Ⅱ) atom is located at the center of a distorted trigonal bipyramid of five coordination atoms (two nitrogen and three chlorine atoms). Two copper(Ⅱ) atoms were bridged by two chlorine anions (Cl(2) and Cl(2a)) to form a Cu(Ⅱ)-Cu(Ⅱ) binuclear entity with the distance between two copper(Ⅱ) atoms of 3.398 (A).     

H2在Cu/ZnO/Al2O3型低变催化剂上的TPD研究

采用TPD法研究了H₂在Cu/ZnO/Al₂O₃上的脱附动力学,结果表明在350℃以内,Cu/ZnO/Al₂O₃对H₂显示出具有不同能量特征的两个活泼部位(Ⅰ)、(Ⅱ),借助于脱附速率等温线法对(Ⅰ)、(Ⅱ)进行解析,建立了相应的脱附速率方程,并发现Cu/ZnO/Al₂O₃对H₂的有效表面为非理想表面,(Ⅰ)、(Ⅱ)对有效表面积的贡献分别为27.6%及72.4%。     

半胱氨酸铜络合物的生成及其结构的研究

本文研究了在不同pH值下,半胱氨酸与CuCl_2络合生成的三种不同的络合物。在酸性溶液中,半胱氨酸与CuCl_2通过络合反应、自氧化还原反应,最后生成带氯桥的络合物[Cu_2(Ⅰ)Cl_2(cysH_2)]的白色粉末,(cysH_2为半胱氨酸)。在碱性溶液中,若反应在空气中进行,半胱氨酸与CuCl_2经氧化还原反应,结果生成天蓝色络合物(Cu_2(Ⅱ)(cyss)_2],(cyss~(2-)为胱氨酸根);若反应在绝氧条件下进行,它们则先络合,然后二聚成黑色络合物[Cu_2(Ⅱ)(cys)_2·6H_2O)。根据化学分析以及IR和ESR谱的研究,推测了这三种络合物的可能结构。     

STUDY ON DETERMINATION OF TRACE Cu（Ⅱ） BY DDCT CHELATING RESIN PRECONCENTRATION AND THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A new method for determination of Cu(Ⅱ) by DDCT chelating resin preconcentration and thin layer resin phase spectrophotometry was developed. The method has a high sensitivity (ε435 =3.6×105 L/mol· cm), which is 33 times higher than that of liquid phase spectrophotometry. It has a good selectivity (most coexisting ions could not influence determination) and an ideal precision [30μg Cu(Ⅱ), n=6, RSD= 1.67%]. The content of Cu(Ⅱ) in water, high purity rare earth and its oxide was determined. The detection limit of Cu(Ⅱ) is 5.3μg/L, and the linear range is 0～7.2 μg/ml. The result is satisfactory.     

Cu(I)Y分子筛的固态离子交换制备及其表征

应用ＩＲ、ＭＳ和ＥＰＲ表征ＣｕＣｌ和ＮＨ４Ｙ固态离子交换过程以及制备Ｃｕ（Ｉ）Ｙ的一些特性。固态离子交换程度依赖于反应温度。和还原Ｃｕ（ＩＩ）Ｙ的方法，固态离子交换是更为有效的制备纯Ｃｕ（Ｉ）Ｙ的方法。     

表面活性剂增敏动力学光度法测定痕量铜

建立了以表面活性剂为增敏剂,过氧化氢还原中性红褪色催化光度法测定痕量铜的新方法。找到了反应的最佳条件,并测定了一些动力学参数。据此建立了测定痕量铜的催化动力学分析法,线性范围为０－３．２μｇ／２５ｍＬ,检出限为８．２＊１０＾－１１ｇ／ｍＬ。方法具有线性范围宽,干扰离子少的优点,对于人发和指甲中铜的测定,结果满意。     

CO在Cu/ZnO上吸附的簇模型研究

采用DFT方法和HF方法对CO在Cu／ZnO催化剂上的Zn（Ⅱ）和Cu（Ⅰ）表面位上的吸附行为进行了比较研究.结果表明：HF方法给出了较弱的M-CO（M＝Zn（Ⅱ），Cu（Ⅰ））表面吸附键描述，但无法正确预测其强弱顺序，MP2方法与DFT方法则给出与实验事实一致的描述.文章还对CO／铜基催化剂吸附体系的IR光谱进行了合理的理论预测.     

The Study of Indirect Determination of Tiopronin by Extraction Flotation Copper(II) with an Ammonium Sulfate‐Water‐n‐Propyl Alcohol System

A novel method for indirect determination of tiopronin by extraction flotation of copper(II) with an ammonium sulfate‐water‐n‐propyl alcohol system was developed. The effects of different parameters, such as acidity, the amount of NH₄SCN and various salts on the flotation yield of Cu(II), have been studied to optimize the experimental conditions. Under the optimum conditions, Cu(II) is reduced to Cu(I) by tiopronin, and the resulting Cu(I) can react with SCN^? to form a white emulsion precipitate CuSCN. In the presence of (NH₄)₂SO₄, the mixture consisting of n‐propyl alcohol and water can be separated into an n‐propyl alcohol phase and a water phase. In the process of phase separation of n‐propyl alcohol from water, the precipitated CuSCN is extracted and stays in the interface of n‐propyl alcohol and water. The amount of tiopronin can be determined by measuring the flotation yield of Cu(II). The detection limit is 0.32 mg L^?1 and the linear range is maintained in the range of 0.40±13.0 mg L^?1 with a correlation coefficient of 0.9991. This proposed method has been successfully applied to the determination of tiopronin in tablets, urine and human plasma with satisfactory results.     

离子液体中铜的电沉积行为

在含有氯化铜的氯化1-丁基-3-甲基咪唑(BMIC)和乙二醇(EG)体系中研究金属铜的电沉积。 在BMIC中加入EG,分别研究了EG对离子液体BMIC的粘度和电导率的影响,并通过循环伏安法研究了BMIC-CuCl2-EG溶液中Cu(Ⅱ)的电化学行为,考察了乙二醇浓度、温度和扫描速度对Cu(Ⅱ)电化学行为的影响。 结果表明,Cu(Ⅱ)的电还原过程分为两个过程,其中Cu(Ⅱ)/Cu(Ⅰ)是扩散控制下的不可逆过程,Cu(Ⅰ)/Cu是不可逆过程。 计算得出,在343 K时,Cu(Ⅱ)/Cu(Ⅰ)还原过程中的扩散系数D为7.0×10-7 cm2/s,传递系数为0.24。 在Cu膜表面进行了电沉积,获得金属铜颗粒,经扫描电子显微镜观察Cu的电沉积层的形貌发现,在343 K时沉积30 min后,金属铜晶粒致密,将沉积时间延长至2 h后,晶粒呈球状。     

用DL-半胱氨酸盐作螯合滴定释放剂的研究和应用

提出以DL-半胱氨酸盐（DL-Cysteine）作释放剂，选择性螯合滴定法测定铜或锡、汞和铊．方法是基于先用EDTA螯合铜（Ⅱ）或锡（Ⅳ）、汞（Ⅱ）、铊（Ⅲ）和其它金属离子，然后用DL-Cysteine解蔽．其它金属离子均不干扰。在测定条件下．试剂（DL－Cysteine）不与大量其它金属-ED-TA配合物起反应。此法已经用于测定各种合金和矿样中的铜或锡、汞和铊，结果令人满意。     

Simple and rapid GLC method for the determination of orphenadrine in human plasma

A rapid and specific method has been developed for the determination of orphenadrine concentration in plasma. It involves a one-step sample preparation using n-hexane/isopropyl alcohol (98:2) extraction, and analysis by gas chromatography on a wide bore capillary column using nitrogen/phosphorus detection. This procedure considerably simplifies previously reported assays and is specific and sensitive enough for the determination of orphenadrine in plasma of patients on chronic therapy.     

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex [Cu(C13H9N2O)Cl]2·(CH3CN)2 with Ligand 2-Benzimidazol

A new dinuclear copper complex, [Cu(C13H9N2O)Cl]2·(CH3CN)2 (C30H24Cl2Cu2N6O2),has been synthesized and characterized by X-ray structure determination. It crystallizes in the triclinic system, space group P1-, with a = 7.6677(14), b = 9.2375(17), c = 11.227(2) (A), α = 81.338(3),β= 88.173(4), γ = 66.199(3)°, V = 718.9(2) (A)3, Z = 1, Mr = 698.53, F(000) = 354, Dc = 1.613 g/cm3,μ(MoKα) = 1.705 mm-1, the final R = 0.0645 and wR = 0.1364 for 2474 unique reflections with 1809 observed ones (I＞ 2σ(Ⅰ)). In the title complex, each copper(Ⅱ) atom is located at the center of a distorted tetrahedron consisting of four coordinate atoms (one nitrogen atom, two oxygen anions,and one chlorine atom). Two copper(Ⅱ) atoms are bridged by two oxygen anions (O(1) and O(1a)) of two phenolates to form a Cu(Ⅱ)-Cu(Ⅱ) binuclear entity, and the distance between two copper(Ⅱ)atoms is 3.0144(15) (A).     

烟气中二氧化硫及三氧化硫测定方法的研究

本文采用过氧化氢-氯化钡-钍试剂法以及80%异丙醇-氯化钡-钍试剂法分别测定了烟气中的二氧化硫及三氧化硫质量浓度,并对该方法的灵敏度、准确度以及各种影响因素进行了研究分析.本方法简单、快速、准确、便于现场监测控制.     

新型杂环三氮烯荧光试剂1,8-双(2-苯并噻唑重氮氨基)萘的合成及其分析应用

将1,8-萘二胺和苯并噻唑类试剂结合, 并引入杂环三氮烯结构, 合成了新荧光试剂1,8-双(2-苯并噻唑重氮氨基)萘(BBTANP), 其结构经红外光谱、核磁共振谱和元素分析证实. 研究结果表明, 在碱性介质中, 该试剂与Cu(Ⅱ)形成1∶1的络合物, 并在λex/λem=362 nm/459 nm处产生荧光增强作用. 据此建立了BBTANP测定Cu(Ⅱ)的新型荧光分析法, 该方法的线性范围为8.0×10-7—1.0×10-5 mol /L, 检测限为1.3×10-7 mol/L. 将其应用于水样中Cu(Ⅱ)的测定, 结果令人满意.     

电化学诱导咪唑铜配合物断裂DNA的研究

二价咪唑铜配合物可以在电极表面发生氧化还原反应,该过程对应于单电子准可逆过程.荧光光谱电化学结果表明,还原产物一价咪唑铜配合物可以被空气中的O₂氧化为二价.在中性的Tris-HCl缓冲溶液中,配合物与DNA之间存在弱相互作用,其键合常数仅为2.7×10²L/mol.荧光光谱及电化学结果表明为嵌入式作用.据此建立了一种电化学诱导咪唑铜配合物对DNA断裂的新方法,并采用差示扫描量热(DSC)法检验了断裂结果.     

分光光度法测定新鲜蔬菜中维生素C的含量

水溶性的维生素C是一种人体必需的营养物质。维生素C是含有烯二醇基的多羟基内酯结构,利用其水溶液在波长265nm处有较强烈的紫外吸收峰,建立了直接用紫外分光光度法测定新鲜蔬菜中维生素C含量的方法。实验结果表明,维生素C的含量在1.0¹2.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%12.0μg/mL内线性关系良好,线性方程为A=0.066 03c+0.019 74(R2=0.997 51),检出限为0.044μg/mL,样品加标回收率为97.5%¹05.4%。方法操作简单,准确度高,对新鲜蔬菜的测定结果令人满意。