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机构地区:[1]河北师范大学化学与材料科学学院,石家庄050024
出 处:《中国药房》2017年第15期2089-2092,共4页China Pharmacy
基 金:国家自然科学基金资助项目(No.81173496;20975029)
摘 要:目的:采用三维荧光光谱结合交替三线性分解(ATLD)算法测定徐长卿药材中丹皮酚的含量。方法:构建三线性模型,利用最小二乘原理进行ATLD,采用核一致诊断法对体系的组分数进行拟合,采用数学校正法校正内滤光效应。三维荧光光谱扫描条件:激发波长范围为250~400 nm,发射波长范围为410~600 nm,波长间隔为5 nm,狭缝宽度为5.0/5.0 nm,扫描速度为1 200nm/min;测定吸收光谱条件:扫描波长范围为250~600 nm,扫描速度为600 nm/min;以Al(Ⅲ)作敏化剂增强丹皮酚的荧光强度。以高效液相色谱法(HPLC)测定药材样品中丹皮酚含量作为验证。结果:丹皮酚检测质量浓度线性范围为0.132~1.188μg/m L(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率为100.1%~104.7%(RSD=2.39%,n=9);丹皮酚的解析光谱与其真实光谱几乎完全重合。HPLC测定结果与ATLD算法结果十分相近。结论:三维荧光光谱结合ATLD算法简便、快速、高效、准确,可用于复杂体系中特定组分的定性与定量分析。OBJECTIVE: To determine the content of paeonol in Cynanchum paniculatum by three-dimensional fluorescence coupled with ATLD algorithm. METHODS: The trilinear model was established. The principle of least square was used for ATLD. The component value was fitted by core consistency diagnosis, and inner filter effect was corrected by mathematical correction method. Fluorescence scanning condition included excitation wavelength of 250-400 nm, emission wavelength of 410-600 nm, wavelength interval of 5 nm, slit width of 5.0/5.0 nm, scanning speed of 1 200 nm/min. Determination and absorption spectrum condition included scanning wavelength of 250-600 nm, scanning speed of 600 nm/min; AI( Ⅲ ) was used as the sensitizer to increase the fluorescence intensity of paeonol. The content of paeonol was determined by HPLC. RESULTS: The linear range of paeonol was 0.132-1.188 μg/mL(r=0.999 9). RSDs of precision, stability and reproducibility tests were less than 3.0%. The recoveries were 100.1%-104.7 % (RSD = 2.39 %, n = 6). The analysis spectrum of paeonol was almost completely overlapped with the actual spectrum. The results of HPLC method are very similar to those of ATLD algorithm. CONCLUSIONS: The three-dimensional fluorescence coupled with ATLD algorithm is simple, rapid, efficient and accurate, and can be used for the qualitative and quantitative analysis of complex system.
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