New HPLC method was developed for determination of amlodipine and valsartan in their binary mixture as a part of routine control of combined formulations. The method was validated to meet official requirements includi...New HPLC method was developed for determination of amlodipine and valsartan in their binary mixture as a part of routine control of combined formulations. The method was validated to meet official requirements including selectivity, stability, linearity, precision and accuracy. Chromatography was carried out using a LiChrospher RP-18 column, a mixture containing acetonitrile, phosphate buffer of pH 3.5 and methanol (45:45:10, v/v/v) and new fluorescence detection at 255 nm for excitation and 448 nm for emission. The effect of methanol content, pH of the buffer, flow rate, detection wavelengths and column temperature was estimated in robustness study, according to a plan defined by the Plackett-Burman design. For identification of significant effects, both graphical and statistical methods were used. Ro-bustness for dissolution test was checked estimating the effects of paddle speed, temperature and pH of dissolution medium. The method was proved to complying with all official guidelines. Therefore, it is suitable for determination of amlodipine and valsartan in their binary mixtures for different analytical and pharmaceutical purposes.展开更多
为了建立水禽细小病毒(WPV)快速检测方法,根据序列比对结果在水禽细小病毒NS基因SF3保守区域内设计特异性引物,建立SYBR Green Ⅰ荧光定量PCR通用检测方法。该方法的扩增效率(E)为90.0%,相关系数(R~2)=0.99,标准曲线方程为y=-3.607x+38....为了建立水禽细小病毒(WPV)快速检测方法,根据序列比对结果在水禽细小病毒NS基因SF3保守区域内设计特异性引物,建立SYBR Green Ⅰ荧光定量PCR通用检测方法。该方法的扩增效率(E)为90.0%,相关系数(R~2)=0.99,标准曲线方程为y=-3.607x+38.77;除WPV出现S形扩增曲线外,新城疫病毒(NDV)、H9亚型禽流感病毒(H9 AIV)、鸭坦布苏病毒(DTMUV)、鸭肝炎病毒(DHAV)、鸭肠炎病毒(DEV)、鸭呼肠孤病毒(DRV)样品均未出现S形阳性扩增曲线;批内变异系数(CV)为0.15%~0.23%,批间变异系数为0.09%~0.28%。结果表明,SYBR Green Ⅰ荧光定量PCR检测方法重复性好、灵敏度高和特异性强。临床样品检测结果表明,SYBR Green Ⅰ荧光定量PCR与普通PCR的符合率达98.4%,灵敏度是普通PCR的1 000倍。SYBR Green Ⅰ荧光定量PCR检测方法不仅能定性检测WPV,还可以进行定量检测,可用于种鸭场、种鹅场的WPV净化检测,也可用于WPV临床大量样品的快速检测。展开更多
金属离子过量使用会造成环境污染,危及人类健康。因此,对相关金属离子进行检测显得尤为重要。发光金属有机框架(Luminescent metal-organic frameworks,LMOFs)因其具备高色纯度、超高孔隙率和可调结构等优势,被视为简单有效且有前途的...金属离子过量使用会造成环境污染,危及人类健康。因此,对相关金属离子进行检测显得尤为重要。发光金属有机框架(Luminescent metal-organic frameworks,LMOFs)因其具备高色纯度、超高孔隙率和可调结构等优势,被视为简单有效且有前途的荧光传感材料。本文以3,5-二(4-咪唑-1-基)吡啶(Bip)为主配体,1,4-萘二甲酸(1,4-ndc)为辅助配体,Ni^(2+)为中心离子,采取溶剂热法合成了一例二维金属有机框架[Ni_(2)(Bip)_(2)(1,4-ndc)_(2)(H_(2)O)_(6)](记为CUST-756,其中CUST是Changchun University of Science and Technology缩写),并通过合成后修饰法制备了Eu^(3+)@CUST-756复合发光材料。利用XRD、FT-IR和XPS对合成的CUST-756和Eu^(3+)@CUST-756复合材料进行了基础表征。并且采用荧光光谱对样品进行了发光特性、金属离子传感性能及其机理研究。实验结果表明,Eu^(3+)@CUST-756在甲醇溶液中具备优异的发光性能和良好的稳定性,Eu^(3+)的引入使得材料可用于金属阳离子Cr^(3+)、Fe^(3+)检测。Cr^(3+)离子的检出限(limit of detection,LOD)为5.44µmol·L^(-1);Fe^(3+)离子的LOD为7.51µmol·L^(-1),与大多数LMOFs性能相近。展开更多
以尼龙66(PA66)和植酸(IP6)为前驱体、乙酸为溶剂,采用溶剂热法制备了PA66基碳点(66CDs)。利用TEM、FTIR、XPS、荧光光谱对其进行了表征,对其光学性能、离子稳定性和时间稳定性进行了测试,探究了其指纹识别、荧光防伪、光线阻挡的应用...以尼龙66(PA66)和植酸(IP6)为前驱体、乙酸为溶剂,采用溶剂热法制备了PA66基碳点(66CDs)。利用TEM、FTIR、XPS、荧光光谱对其进行了表征,对其光学性能、离子稳定性和时间稳定性进行了测试,探究了其指纹识别、荧光防伪、光线阻挡的应用。结果表明,将1.6 g PA66、1.1 g IP6加入20 mL乙酸中,于260℃下反应36h,制备的66CDs具有最大荧光强度。66CDs为球形结构,平均粒径4.00nm,表面含有羧基、羟基、氨基等官能团;66CDs的荧光为非激发波长依赖型,最佳激发波长和发射波长分别为360和490 nm,荧光量子产率可达11.69%,其荧光强度不受常见金属阳离子影响,30 d内具有稳定性。由66CDs与水溶性淀粉制备的荧光粉末可用于指纹识别,不仅可将66CDs制成油墨用于荧光防伪,还可将其制成防蓝光膜,用于蓝光防护。展开更多
文摘New HPLC method was developed for determination of amlodipine and valsartan in their binary mixture as a part of routine control of combined formulations. The method was validated to meet official requirements including selectivity, stability, linearity, precision and accuracy. Chromatography was carried out using a LiChrospher RP-18 column, a mixture containing acetonitrile, phosphate buffer of pH 3.5 and methanol (45:45:10, v/v/v) and new fluorescence detection at 255 nm for excitation and 448 nm for emission. The effect of methanol content, pH of the buffer, flow rate, detection wavelengths and column temperature was estimated in robustness study, according to a plan defined by the Plackett-Burman design. For identification of significant effects, both graphical and statistical methods were used. Ro-bustness for dissolution test was checked estimating the effects of paddle speed, temperature and pH of dissolution medium. The method was proved to complying with all official guidelines. Therefore, it is suitable for determination of amlodipine and valsartan in their binary mixtures for different analytical and pharmaceutical purposes.
文摘为了建立水禽细小病毒(WPV)快速检测方法,根据序列比对结果在水禽细小病毒NS基因SF3保守区域内设计特异性引物,建立SYBR Green Ⅰ荧光定量PCR通用检测方法。该方法的扩增效率(E)为90.0%,相关系数(R~2)=0.99,标准曲线方程为y=-3.607x+38.77;除WPV出现S形扩增曲线外,新城疫病毒(NDV)、H9亚型禽流感病毒(H9 AIV)、鸭坦布苏病毒(DTMUV)、鸭肝炎病毒(DHAV)、鸭肠炎病毒(DEV)、鸭呼肠孤病毒(DRV)样品均未出现S形阳性扩增曲线;批内变异系数(CV)为0.15%~0.23%,批间变异系数为0.09%~0.28%。结果表明,SYBR Green Ⅰ荧光定量PCR检测方法重复性好、灵敏度高和特异性强。临床样品检测结果表明,SYBR Green Ⅰ荧光定量PCR与普通PCR的符合率达98.4%,灵敏度是普通PCR的1 000倍。SYBR Green Ⅰ荧光定量PCR检测方法不仅能定性检测WPV,还可以进行定量检测,可用于种鸭场、种鹅场的WPV净化检测,也可用于WPV临床大量样品的快速检测。
文摘金属离子过量使用会造成环境污染,危及人类健康。因此,对相关金属离子进行检测显得尤为重要。发光金属有机框架(Luminescent metal-organic frameworks,LMOFs)因其具备高色纯度、超高孔隙率和可调结构等优势,被视为简单有效且有前途的荧光传感材料。本文以3,5-二(4-咪唑-1-基)吡啶(Bip)为主配体,1,4-萘二甲酸(1,4-ndc)为辅助配体,Ni^(2+)为中心离子,采取溶剂热法合成了一例二维金属有机框架[Ni_(2)(Bip)_(2)(1,4-ndc)_(2)(H_(2)O)_(6)](记为CUST-756,其中CUST是Changchun University of Science and Technology缩写),并通过合成后修饰法制备了Eu^(3+)@CUST-756复合发光材料。利用XRD、FT-IR和XPS对合成的CUST-756和Eu^(3+)@CUST-756复合材料进行了基础表征。并且采用荧光光谱对样品进行了发光特性、金属离子传感性能及其机理研究。实验结果表明,Eu^(3+)@CUST-756在甲醇溶液中具备优异的发光性能和良好的稳定性,Eu^(3+)的引入使得材料可用于金属阳离子Cr^(3+)、Fe^(3+)检测。Cr^(3+)离子的检出限(limit of detection,LOD)为5.44µmol·L^(-1);Fe^(3+)离子的LOD为7.51µmol·L^(-1),与大多数LMOFs性能相近。
文摘以尼龙66(PA66)和植酸(IP6)为前驱体、乙酸为溶剂,采用溶剂热法制备了PA66基碳点(66CDs)。利用TEM、FTIR、XPS、荧光光谱对其进行了表征,对其光学性能、离子稳定性和时间稳定性进行了测试,探究了其指纹识别、荧光防伪、光线阻挡的应用。结果表明,将1.6 g PA66、1.1 g IP6加入20 mL乙酸中,于260℃下反应36h,制备的66CDs具有最大荧光强度。66CDs为球形结构,平均粒径4.00nm,表面含有羧基、羟基、氨基等官能团;66CDs的荧光为非激发波长依赖型,最佳激发波长和发射波长分别为360和490 nm,荧光量子产率可达11.69%,其荧光强度不受常见金属阳离子影响,30 d内具有稳定性。由66CDs与水溶性淀粉制备的荧光粉末可用于指纹识别,不仅可将66CDs制成油墨用于荧光防伪,还可将其制成防蓝光膜,用于蓝光防护。
