摘要
目的：建立固相萃取（SPE）净化后紫外分光光度法（UV）快速测定黄花蒿中青蒿素含量。方法：黄花蒿干叶粉末中的青蒿素用无水乙醇超声波提取（200 W,40 k Hz）,最佳提取条件为料液比1∶20（g∶mL）,超声波萃时间15 min,温度25℃。提取液0.05 mol·L^-1氢氧化钠水溶液45℃衍生20 min。衍生化后经C18SPE柱净化,乙醇-0.01 mol·L^-1磷酸盐缓冲液（p H 5.8）（15∶85）洗涤杂质,乙醇-0.01 mol·L^-1磷酸盐缓冲液（p H5.8）（33∶67）洗脱青蒿素衍生物Q259。洗脱液用紫外分光光度计259 nm波长处测定。结果：经高效液相色谱（HPLC）检测,SPE净化后Q259回收率在98.0%～105.9%;Q259对λ259光吸收贡献从26.8%～53.5%提高到92.0%～100%,λ259有光吸收的杂质基本除去;SPE-UV法与HPLC法相对误差小于10%。结论：SPE-UV法经方法学验证,可作为黄花蒿种植、收购时大量、快速检测黄花蒿中青蒿素含量的检测方法。
Objective： To establish a method for rapid determination of artemisinin in Artemisia annua L. using solid phase extraction（ SPE） followed by UV-spectrophotometry. Methods： Artemisinin was extracted from A. annua using anhydrous ethanol as the extracting solvent by ultrasonic wave（ 200 W,40 k Hz）. The optimal extraction condition was as follows： the solid-liquid ratio 1∶ 20（ g∶ mL）,the extraction time 15 minutes at 25 ℃. The extraction solution was derivatized in 0. 05 mol·L^-1 Na OH solution for 20 min at 45 ℃. The sample was purified by C18 SPE column with ethanol-0. 01 mol·L^-1 phosphate buffer（ p H5. 8）（ 15∶ 85）,eluted by ethanol-0. 01 mol·L^-1 phosphate buffer（ p H 5. 8）（ 33∶ 67） and detected by UV-pectrophotometry at 259 nm. Results： The recovery rate of Q259 was between 98. 0% and 105. 9% after purifying by SPE which was detected by HPLC. And the contribution of Q259 for light absorption in λ259improved from 26. 8%-53. 5% to 92. 0%-100%,which indicated that the impurities absorbed in λ259were almost removed. The relative error between SPE-UV and HPLC was less than 10%.Conclusion： The SPE-UV after verification methodology could work effectively in on-site rapid determination of arteannuin content in large quantity of A. annua during planting and purchasing.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第2期255-260,共6页
Chinese Journal of Pharmaceutical Analysis
基金
地方高校国家级大学生创新创业训练计划项目(201310399007)
