基于中空纤维液相微萃取的黄酮类化合物测定

摘要

目的 建立中空纤维液相微萃取(HFLPME)-高效液相色谱法(HPLC)测定中药侧柏中黄酮类化合物含量.方法 以聚偏氟乙烯为有机溶剂载体,正己醇为接受相,10-5 mol/L HCl为供相,在1 500 r/min搅拌下萃取45 min,萃取结束后,蒸干接受相中有机溶剂,用50 μl甲醇溶解后进行HPLC分析.结果 分析物二氢杨梅素、杨梅素、漆黄素、槲皮素、柚皮素、山柰素、异鼠李素和白杨素在0.01-10.0 μg/ml范围内线性关系良好;检出限为0.01-1.0 ng/ml;平均浓缩因子在5.4-30.6倍之间;中药侧柏中分析物的平均回收率为97.5%.结论 HFLPME操作简单、快速、有机溶剂用量少、富集倍数高、对测定中药中微量或痕量黄酮类有效成分具有重要的意义.%Objective To e.stablish a hollow fiber liquid phase microextraction ( HFLPME ) coupled with high performance liquid chromatography ( HPLC ) for determining the contents of the flavonoids in Platycladu.s orientalis. Methods The analytes were extracted under 1 500 r/min agitation for 45 min with polyvinylidene difluoride as the organic solvent supporter,l0-5 mol/L HCl as the donor phase , and n-hexanol as the acceptor phase. After extraction, the organic solvent in the acceptor phase was dried , and then dissolved with 50 μl methanol. The analytes were determined by HPLC. Results The analytes showed a good linear relationship by HFLPME-HPLC in the range of 0. 01 - 10. 00μg/ml. The limits of detection were 0. 01 - 1. 0 ng/ml. The enrichment fac:tors of flavonoids ingredients ranged from 5. 4 to 30. 6. The average recovery of analytes in Platycladu.s orientalis was 97. 5％ . Conclusion The method is simple,rapid, and effective. It has a great significance on the analysis of trace flavonoid compounds in traditional Chinese medicine.