西咪替丁与氯醌酸荷移反应的研究

研究了西咪替丁与氯醌酸的荷移反应。确定了形成电荷转移络合物的最佳反应条件。在丙酮介质中,电子给体西咪替丁与电子受体氯醌酸于室温下可形成1：1的荷移络合物,络合物的最大吸收波长为516.6nm;表观摩尔吸光系数ε=2.22×103L.mol-1.cm-1;线性范围为6.8—112.0μg/mL;相关系数r为0.9995;并对形成荷移络合物的反应机理进行了探讨,并应用拟定的方法对样品西咪替丁片剂进行了含量测定,回收率为99.44%—100.20%;RSD为1.3%。     

克拉霉素与醌茜素的荷移反应及其测定

克拉霉素与醌茜素在乙醇 -水介质中发生电荷转移反应 ,形成 1∶ 1的电荷转移络合物。该络合物在5 80 nm处有最大吸收 ,表观摩尔吸光系数为 3.74× 1 0 3 L·mol-1· cm-1 ,稳定常数是 2 .6× 1 0 5。建立了一种快速测定克拉霉素的荷移分光光度法。药物浓度在 0— 1 0 0 mg/ L范围内服从比耳定律。本法测定了克拉霉素制剂中有效成分的含量 ,与文献法结果基本吻合。     

奥美拉唑与氯冉酸的荷移反应及其测定

奥美拉唑 (电子给予体 )与氯冉酸 (电子接受体 )在丙酮介质中生成 1∶ 1型荷移络合物 ,在波长5 2 5 nm处有最大吸收 ,表观摩尔吸光系数是 1.0 2× 10 3 L· mol-1·cm-1。依据此荷移反应建立了一种快速测定奥美拉唑的荷移分光光度法。药物浓度在 2 0— 30 0 mg/ L范围内服从比耳定律。 6次测定结果的相对标准偏差为 0 .4 8% ,利用本法测定了奥美拉唑胶囊中有效成分的含量 ,结果令人满意。     

甲磺酸培氟沙星与氯冉酸的荷移反应

利用甲磺酸培氟沙星与氯冉酸在甲醇介质发生荷移反应,建立了荷移分光光度法测定甲磺酸培氟沙星含量的方法。结果表明,荷移反应生成1∶1型配合物,最大吸收波长为530nm,甲磺酸培氟沙星线性范围为2.25×10-8—3.38×10-6mol/L浓度内,回收率为98.7%—101.4%。     

用吐温80-硫酸铵-水体系的液-固萃取光度法测定痕量镍

研究了Ni()-PAR在吐温80-硫酸铵-水体系中的最佳萃取条件,建立了水样中测定痕量镍的非有机溶剂液-固萃取光度法。在NH3·H2O-NH4Cl缓冲溶液中,金属配合物Ni()-PAR可被吐温80固相富集萃取,最大吸收波长为500nm,镍含量在0—1.0μg/mL范围内服从朗伯-比耳定律,表观摩尔吸光系数为6.345×104L·mol-1·cm-1。该法测定水样中镍含量,回收率可达96.3%—103.0%。     

对硝基酚分光光度法测定氯氮卓的含量

本文主要研究在硼砂水溶液中 ,氯氮卓与对硝基酚发生荷移反应 ,生成稳定的 1∶ 1络合物。络合物的最大吸收波长为 4 35 nm,表观摩尔吸光系数 ε=3.83× 10 3L·mol-1·cm-1。基于以上反应 ,本方法测定氯氮卓药物制剂含量与文献值基本一致 ,回收率为 99.61%— 10 0 .10 % ,相对标准偏差为 0 .64%     

替米沙坦与氯冉酸的荷移反应

用分光光度法研究了替米沙坦与氯冉酸的电荷转移反应条件,替米沙坦与氯冉酸在丙酮溶液中可以发生电荷转移反应,在室温下按实验方法配好溶液即可比色。电荷转移络合物的最大吸收波长是525nm,表观摩尔吸光系数为2.18×10²L·mol^-1·cm^-1。替米沙坦质量浓度在16—192mg·L^-1范围内服从比耳定律,相关系数为0.9997。当替米沙坦浓度为80mg·L^-1时,六次测定结果的相对标准偏差为1.33%,回收率在99.0%以上。测得荷移络合物的组成和稳定常数分别为1:2和3.9×10⁷。用于测定制剂中替米沙坦的含量结果令人满意。     

一种可用于酚类化合物检测的酶传感器

利用溶胶-凝胶法将辣根过氧化物酶(HRP)固定化于二氧化硅凝胶网络中构建了可用于酚类化合物检测的酶传感器。对二氧化硅载体材料进行了结构表怔。二氧化硅多孔材料的平均孔径为2.95 nm。孔径小于5 nm占总数的84.068%。由于辣根过氧化物酶的分子尺寸远远大于二氧化硅的凝胶网络的平均孔径,因此不会泄露到溶液中去,而尺寸较小的底物可以发生反应。包埋的辣根过氧化物酶在H₂O₂的存在下,能够催化氧化苯酚与4-氨基安替比林反应生成醌亚胺有色化合物。通过紫外-可见光谱测定醌亚胺有色化合物的吸光度,即可以确立苯酚的含量。对于象含氯酚类的重要污染物, 如邻氯酚、间氯酚、2,4-二氯酚,这种方法也同样适用。此外,对多次测定以后的酶的活性下降的问题进行了讨论,结果表明酶传感器可以重复使用10次以上。但响应时间会变长。     

荷移反应用于对氨基水杨酸钠的测定

本研究了对氨基水杨酸与２，６－二氯醌氯亚胺的荷移反应，确定了反应条件，反应在丙酮介质中进行，二形成１：１的络合物，其最大吸收波长为６６０ｎｍ，表观摩尔吸光系数为１．１７×１０＾３Ｌ．ｍｏｌ．ｃｍ＾－１，用拟定方法测定对氨基水杨酸钠制剂的含量，获得满意的结果。     

离子对-反相高效液相色谱法同时测定解磷注射液中氯磷定、盐酸苯那辛、硫酸阿托品的含量

研究建立了离子对 -反相高效液相色谱法 ( IP- HPLC)同时测定解磷注射液中氯磷定、硫酸阿托品、盐酸苯那辛含量的分析方法及其有关物质和降解产物检查法。采用 ZORBAXSB C18色谱柱 ,流动相 :甲醇 -乙腈 - 1mol· L-1磷酸 (用三乙胺调 p H=3.0 ) - 0 .2 mol· L-1磷酸二氢钠 (用磷酸调 p H=3.0 ) - 0 .9%十二烷基硫酸钠水溶液 ( 2 0 0∶ 4 0 0∶ 10∶ 90∶ 30 0 ) ,在流速 1.0 m L· min-1下 ,检测波长 2 2 0 nm处 ,测定氯磷定、硫酸阿托品、盐酸苯那辛 ,其回收率分别为 10 0 .36% ( RSD 0 .90 % )、99.4 4 % ( RSD 1.0 9% )、99.82 %( RSD 1.2 3% )。该方法简便、快速 ,适用于制剂中各组分含量的同时测定     

Fiber-optic sensor based on evanescent wave absorbance around 2.7 μm for determining water content in polar organic solvents

The feasibility of sapphire fiber-optic sensors based on evanescent wave absorption spectroscopy in the infrared range for quantitative determination of water content in polar organic solvents has been investigated. Evanescent wave absorption spectra of sapphire fiber-optic sensors in glycerol, ethanol, and glycol with different water concentrations obtained and analyzed, respectively. Evanescent absorbance of the sensors in those organic solvents has been utilized to implement for in situ monitoring water concentration in organic solvents. The evanescent absorbance of sensors in glycerol and glycol has been found to vary linearly with water content in the range 0–30 % and in ethanol in the range 0–10 %, respectively. The fiber-optic sensors based on evanescent absorbance for monitoring water concentrations in those organic solvents are acceptably accurate, cost-effective, and reliable. Some methods to improve the accuracy of predicated water content in those organic solvents are also suggested. Overall, the results demonstrate that the sapphire fiber-optic sensor based on evanescent absorption spectroscopy is a promising candidate for prediction of water content in polar organic solvents in on-line and remote situation.     

析相光度法测定铁(Ⅲ)的研究

本研究了铁（Ⅲ）－ＰＥＧ（聚乙二醇－２０００）－铬锖Ｒ－Ｎａ２ＳＯ４体系的上光度法并应用于测定Ｆｅ（Ⅲ）。最适酸并为４．５￣６．５（ＮａＡｃ－ＨＡｃ）缓冲溶液,其络合物的最大吸收位于５６０ｎｍ,表观摩尔吸光系数为５．３６×１０＾４Ｌ·ｍｏｌ＾－１·ｃｍ＾－１,Ｆｅ（Ⅲ）浓度在０￣４μｇ范围内服从比尔定律,铁与铬菁Ｒ形成组成为１：２的稳定络合物。该方法用于蔡叶中铁的测定,获得了满意的结果。     

新药磺胺嘧啶锌中有机溶剂残留量测定

建立了国家二类新药磺胺嘧啶锌中有机溶剂甲醇和丙酮残留量的毛细管顶空气相色谱分析法。采用PEG-20M弹性石英毛细管色谱柱,F ID检测器,程序升温方法,以氮气为载气。两种有机溶剂完全分离,在浓度范围内具有良好的线性（r均大于0.999）,丙酮和甲醇的检出限分别为3.7m g/L和2.9m g/L,精密度RSD均小于1%,平均回收率分别为101.1%和100.8%.经实验方法学验证,该方法灵敏、准确可靠,适用于磺胺嘧啶锌原料药中有机溶剂残留量的测定。     

A Highly Efficient Turn-On Fluorescent Sensor for Determination of Water in Organic Solvents

2, 3 biphenyl quinoxaline 6-amine is a fluorescent compound in some organic solvents with an excitation wavelength at 435?nm and a fluorescence emission at 518?nm. The fluorescence intensity of 2, 3 biphenyl quinoxaline 6-amine is significantly reduced in the presence of bis-(2, 4, 6-trichlorophenyl) oxalate (TCPO) and Zn(2+) due to the nonfluorescent complex formation. The low stability of the complex in presence of trace amount of water results in decomposing complex, thereby recovering the photoluminescence of 2, 3 biphenyl quinoxaline 6-amine. Based on this fact, a turn-on fluorescence photoluminescence sensor for determination of water content in organic solvents was introduced for the first time.The fluorescence intensity of 2, 3 biphenyl quinoxaline 6-amine as a function of water concentration was used as a simple, sensitive and rapid method for determining trace amount of water in some organic solvents such as ethanol and methanol. The obtained results showed a good linear relationship between fluorescence intensity and the water content with a dynamic range of 0.0094 -1(v/v%), related coefficient of 0.9922 and limit of detection of 0.0026(v/v%). %).     

Fluorescence and Nonlinear Optical Properties of Organic Dye in Inorganic Glass and Xerogel Matrices

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Resonant infrared matrix-assisted pulsed laser evaporation of TiO2 nanoparticle films

The successful development of flexible, high performance thin films that are competitive with silicon-based technology will likely require fabricating films of hybrid materials that incorporate nanomaterials, glasses, ceramics, polymers, and thin films. Resonant infrared matrix-assisted pulsed laser evaporation (RIR-MAPLE) is an ideal method for depositing organic materials and nanoparticles with minimal photochemical or photothermal damage to the deposited material. Furthermore, there are many nonhazardous solvents containing chemical functional groups with infrared absorption bands that are accessible using IR lasers. We report here results of recent work in which RIR-MAPLE has been employed successfully to deposit thin films of TiO₂ nanoparticles on Si substrates. Using an Er:YAG laser (λ=2.94 μm), we investigated a variety of MAPLE matrices containing –OH moieties, including water and all four isomers of butyl alcohol. The alcohol isomers are shown to provide effective and relatively nontoxic solvents for use in the RIR-MAPLE process. In addition, we examine the effects of varying concentration and laser fluence on film roughness and surface coverage.     

Study on the Electrospinnability of Polyvinyl Alcohol Solutions by Using Water/N,N-dimethylacetamide or Water/N,N-dimethylformamide as Solvents

The electrospinning of poly(vinyl alcohol) (PVA) (99% hydrolysis degree) aqueous solution with added organic solvents N, N-dimethylacetamide (DMAc) or N, N-Dimethylformamide (DMF) was investigated. After the addition of the organic solvents to the PVA aqueous solutions, the surface tension and conductivity decreased and the viscosity significantly increased, which caused an improved electrospinnability of the PVA solutions. The micro-structures of the three solutions were investigated by dynamic light scattering (DLS), differential scanning calorimetry (DSC) and dynamic viscoelastic measurements. The DLS data revealed that the swelling of the PVA coils was slightly increased but the overlaps of PVA coils decreased greatly after one of the organic solvents was added to the aqueous solution. The DSC data showed both the water-rich phase and PVA-rich phase were destroyed and the solution became more homogenous after the addition due to the interaction between the organic solvent and water. Viscoelastic data showed there was an obvious difference in the storage modulus behavior between the aqueous solutions and the water/solvents solutions. These changes in the micro-structure and properties were the reason for the improved electrospinnability of the PVA solution. According to scanning electron microscopy (SEM), the average diameter of the electrospun PVA nanofibers was about 308 nm for the DMF/water system, and 255 nm for the DMAC/water system, as compared with uneven diameter nanofibers for the water system.     

利用太赫兹反射式时域光谱系统测量有机溶剂的光学参数

采用太赫兹反射式时域光谱系统,测量了包括正己烷、液状石蜡、无水酒精和水在内的四种有机溶剂的反射式时域光谱,并根据实验模型设计了两种计算方法提取液体样品的光学参数.此外,还将反射算法得到的样品光学参数与透射算法的结果进行比较,验证了反射式系统对应算法结果的正确性,解决了透射系统无法准确测量和提取对太赫兹吸收很强的样品的光...     

Imperviousness of the hydrophobic silica aerogels against various solvents and acids

The experimental results on the imperviousness of the silica aerogels against various organic solvents and acids, are reported. Various types of hydrophobic silica aerogels were prepared using methyltrimethoxysilane (MTMS); tetraethoxysilane (TEOS) with ethyltriethoxysilane (ETES) and phenyltriethoxysilane (PTES) as co-precursors. The organic solvents used were: methanol, ethanol and acetone, and the acids used were: hydrochloric acid (HCl), nitric acid (HNO₃) and sulphuric acid (H₂SO₄). The imperviousness of the aerogels against these solvents and acids were tested with the variation of the percentage of organic solvents and acids in water from 10 to 100% and was characterized by the contact angle measurements. It was observed that in all the cases, the contact angle decreased with an increase in the percentage of solvent in water. While there was no absorption of the solvent up to 20% in water by the ETES and PTES modified aerogels, the MTMS-based aerogels showed the imperviousness up to 60% of the solvent in water. The MTMS aerogels were also impervious against all the three acids up to 100%, while the ETES and PTES modified aerogels could withstand only up to 80% of acids in water.     

激光热透镜光谱法测量有机溶剂的弱吸收

本工作采用反向交叉式双光束激光热透镜光谱法,以氩离子激光作泵浦光源,在514.5nm波长条件下,测量了十五种有机溶剂和水的极小的吸收系数,获得了较高的测量灵敏度。洋细研究了基本实验参数,讨论了光路系统,讨论和比较了测量各类有机溶剂的吸收系数实验结果。