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%.