纳米氧化钛包覆层析硅胶在植物和药物中水杨酸分析的应用

Preparation of Nano Titanium Oxide Coated Silica Gel by Liquid Phase Deposition and Its Use in Analysis of Salicylic Acid in Plants and Medicines

采用液相沉积法制备了纳米TiO。包覆层析硅胶，并将其作为固相萃取（SPE）材料，结合高效液相色谱法（HPLC）测定了药物和植物叶片中水杨酸含量。分别优化了植物和药物中水杨酸的SPE和HPLC分离测定条件，建立了水杨酸的简单快速分析方法。最佳条件下，药物中水杨酸在5～2000ng／mL范围内具有良好线性关系，检出限和定量限分别为1．7、5．7ng／mL，日内和日间测定的相对标准偏差≤14．5％；水稻叶基质中加水杨酸标样在1～100μg／g范围内线性关系良好，检出限和定量限分别为0．17、0．56μg／g，日内和日间测定的相对标准偏差≤14．0％。结果表明，采用液相沉积法制备的纳米TiO2包覆层析硅胶对水杨酸具有较强的萃取性能。所建立的方法简便、灵敏度高，适合于药物及植物中水杨酸的检测。

Titanium nanoparticle（TiO2 NP）-deposited silica gel was prepared by liquid phase deposition （LPD） technique,and used as the solid phase extraction material for the extraction of salicylic acid from plants and medicines. A series of extraction conditions and separation conditions were optimized. A simple, rapid and effective method for the quantitative analysis of salicylic acid in medicines and in plants was established,A linear relatioship was obtained for 5-2 000 ng/mL salicylic acid in medicines. The limit of detection（LOD） and limit of quantification（LOQ） for salicylic acid were 1.7 ng/mL and 5.7 ng/ mL,respectively. Reproducibility of the method was obtained with both intra-day and inter-day relative standard deviations（RSDs） less than 14.5%. The developed method was successfully used to analyze salicylic acid from three medicines. Good linearity was also obtained for 1-100 μg/g salicylic acid spiked in rice with LOD of 0.17 μg/g and LOQ of 0.56 μg/g. Reproducibility of the method was obtained with both intra-day and inter-day relative standard deviations（RSDs） less than 14.0 % and the recoveries in plant samples ranged from 95.3 % to 109.9%.