建立表面增强拉曼光谱法定性定量检测保健食品中非法添加物硝苯地平。采用柠檬酸三钠法制备胶体金,探索最优金胶浓度及粒径范围,确定以100 mL纯水中加入3 mL 1%氯金酸溶液及2.7 mL 1%柠檬酸三钠制备的金胶具备良好的信号增强效果,经粒...建立表面增强拉曼光谱法定性定量检测保健食品中非法添加物硝苯地平。采用柠檬酸三钠法制备胶体金,探索最优金胶浓度及粒径范围,确定以100 mL纯水中加入3 mL 1%氯金酸溶液及2.7 mL 1%柠檬酸三钠制备的金胶具备良好的信号增强效果,经粒径仪结果显示金溶胶粒在85 nm左右。利用拉曼光谱的特异性进行硝苯地平定性检测,结果发现部分降血压药物在(1334±3)cm^(-1)和(1642±3)cm^(-1)处有明显特征峰,用三聚氰胺作为内标物进行硝苯地平定量检测,以硝苯地平特征峰1334 cm^(-1)与三聚氰胺特征峰707 cm^(-1)的峰高比为纵坐标,硝苯地平浓度为横坐标进行线性拟合,结果发现硝苯地平质量浓度在0~100 mg/L有良好线性关系,相关系数为R^(2)=0.9957,定性检测线为5 mg/L,其固体、液体样品加标回收率分别为88.8%~96.5%和90.2%~96.6%,标准偏差分别为4.17%和3.49%。试验方法准确、灵敏、快速,可用于保健品中非法添加硝苯地平药物的定性定量检测。展开更多
目的:研究盐酸金霉素眼膏粒度检验方法,应用显微拉曼光谱法快速鉴定粒子,分析粒度超标原因。方法:应用显微镜法检查盐酸金霉素眼膏粒度;采用显微拉曼光谱法对盐酸金霉素粒子进行快速检测和鉴别,测定条件:532 nm激光器,2.5 m W激光功率,0...目的:研究盐酸金霉素眼膏粒度检验方法,应用显微拉曼光谱法快速鉴定粒子,分析粒度超标原因。方法:应用显微镜法检查盐酸金霉素眼膏粒度;采用显微拉曼光谱法对盐酸金霉素粒子进行快速检测和鉴别,测定条件:532 nm激光器,2.5 m W激光功率,0.002 s曝光时间,1 000次累加。结果:部分企业粒度检查结果不符合标准规定,粒度批间差异较大;由显微拉曼光谱表明样品中超过50μm的微粒均为盐酸金霉素粒子。结论:部分企业生产工艺未对粒度进行有效控制,是导致产品粒度超标的根本原因;建议《中华人民共和国药典》2015年版四部粒度检查法对粒径测定标准等方面做出更详细的规定;显微拉曼光谱法在药品显微鉴别结果准确,具有较好的的应用前景。展开更多
In this paper, nano-porous A1N micro-rods were prepared and characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, Brunauer-Emett-Teller （BET） met...In this paper, nano-porous A1N micro-rods were prepared and characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, Brunauer-Emett-Teller （BET） method of nitrogen adsorption at low temperature, UV-via absorption spectrometry and Raman spectrometry. The SEM images and TEM images showed that the A1N samples were micro-size rods with pores in their surfaces evenly. The length of the rod was in the range of a few mi- crons to tens of micron, the diameter of the rods was about one micron, the diameter of the pore was about hundreds of nano- meter and the wall thickness of the pore about tens of nanometer. The BET surface area of the sample was 41.424 ma/g. The optical spectra showed that the optical properties of the A1N samples almost agreed with that of A1N bulk or film.展开更多
基金supported by the National Natural Science Foundation of Shanxi Provincial Department of Education (Grant No. 2010JK744)the Key Academic Discipline Project of Shaanxi Province
文摘In this paper, nano-porous A1N micro-rods were prepared and characterized by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, Brunauer-Emett-Teller （BET） method of nitrogen adsorption at low temperature, UV-via absorption spectrometry and Raman spectrometry. The SEM images and TEM images showed that the A1N samples were micro-size rods with pores in their surfaces evenly. The length of the rod was in the range of a few mi- crons to tens of micron, the diameter of the rods was about one micron, the diameter of the pore was about hundreds of nano- meter and the wall thickness of the pore about tens of nanometer. The BET surface area of the sample was 41.424 ma/g. The optical spectra showed that the optical properties of the A1N samples almost agreed with that of A1N bulk or film.
