液相微萃取-高效液相色谱法测定银杏叶中槲皮素山柰素和异鼠李素的含量  

Determination of Quercetin,Kaempferol and Isorhamnetin in Ginkgo biloba L. by Nonaqueous Liquid-phase Microextraction with Back Extraction Coupled with High Performance Liquid Chromatography

作　　者：杨雪[1] 白小红[2] 张丽[2] 秦颖[2] 

机构地区：[1]长治医学院药学系药物分析教研室,046000 [2]山西医科大学药学院

出　　处：《长治医学院学报》2012年第1期1-5,共5页Journal of Changzhi Medical College

基　　金：山西省自然科学基金资助项目(2007011086)

摘　　要：目的:利用基于中空纤维为支持体的非水液相微萃取/后萃取-高效液相色谱法同时测定中药银杏叶中槲皮素、山柰素和异鼠李素的含量。方法:对影响萃取富集效率的实验条件进行优化,选定了聚砜纤维长度为10cm,正辛醇为萃取溶剂,含HCl 1×10-3 mol/L的甲醇溶液2.00mL为供相,pH10的NaOH为接受相,以1 500r/min搅拌萃取30min。萃取完成后,取接受相20μL进样高效液相色谱分析。结果:槲皮素、山柰素与异鼠李素的线性范围分别为:0.37～49.87,0.37～49.87和0.19～25.69μg/mL,相关系数均大于0.994。检测限分别为40、70、90ng/mL。平均回收率分别为89.9%～103.4%,101.3%～115.0%,97.3%～107.3%(n=5)。RSD分别为4.6%、3.7%和4.3%。结论:该方法能有效去除复杂基体的干扰,适用于银杏叶中槲皮素、山柰素和异鼠李素的含量测定。Objective.. Nonaqueous liquid-phase microextraction with back extraction （NLPME/BE） based on porous hollow fibers coupled with high performance liquid chromatography （HPLC） was developed for the simultaneous determination of quercetin,kaempferol and isorhamnetin in Ginkgo biloba L.. Methods;The effect of different factors on the extract efficiency were investigated. The optimal experimental conditions, the polysulfone fiber was cut into 10 cm pieces, n-octanol as organic solvent, 1 X 10 3 mol/L HC1 of methanol 2.00 mL as the donor phase, pill0 NaOH as the acceptor phase,1 500 r/min of the stirring rate and 30 min of the extraction time, were selected. An aliquot （20 /~L）, after extraction,was injected into an HPLC system. Results：The linear ranges of quercetin, kaempferol and isorhamnetin were 0. 37-49. 87, 0.37 - 49.87 and 0. 19 - 25.69 /μg/mL, with the correlation coefficient （r） better than 0. 994, limits of detection were 40,70 and 90 ng/ml, respectively. The relative recoveries were 89.9 % - 103.4% /00,101.3 %- 115.0 % and 97.3%-107.3% （ n=5） and the relative standard deviation were 4.6%, 3.7% and 4.3%, respectively. Conclusion：This method was applied to eliminate the interference of multiplicity organism, and results showed the possibility for the determination of quercetin, kaempferol and isorhamnetin in Ginkgo biloba L.

关 键 词：非水液相微萃取/后萃取 槲皮素 山柰素 异鼠李素 银杏叶 

分 类 号：R914.1[医药卫生—药物化学]