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摘要
建立了96-孔板中空纤维膜液相微萃取(HF-LPME)与高效液相色谱(HPLC)联用技术测定槲皮素油水分配系数和不同介质中富集倍数的方法。对96-孔板中空纤维膜液相微萃取条件进行优化,优化后的萃取条件为:60%聚丙烯中空纤维膜,萃取溶剂为正辛醇,振荡速度为173 r/min,萃取温度为室温,样品溶液的pH为4.0,萃取时间为90 min。槲皮素在浓度范围内线性关系良好,相关系数r2≥0.992 3,加样回收率≥93.12%。槲皮素油水分配系数为2.05,在水溶液中的富集倍数高于血清样品中的富集倍数,而血清样品中加入2%甲醇时富集倍数最大。血清样品中加入2%甲醇时槲皮素富集倍数为99.54,是在水溶液中富集倍数156.01的63.8%。该技术快速、简便,灵敏度高,具有广泛的应用前景。
Abstract
A 96-well based hollow fiber liquid phase microextraction (HF-LPME) coupled with HPLC method is developed to determine the oil-water partition coefficient and enrichment factor of quercetin in different media.Conditions for 96-well hollow fiber liquid phase microextraction are optimized as follows:polypropylene hollow fiber has a porosity of 60%,octanol is used as extraction solvent,pH of sample solution is 4,shaking speed is 173 r·min-1,and the extraction performs for 90 min at room temperature.Calibration curves of quercetin show good linear relationship in the concentration range of 0.921-15 mg·L-1,with a recovery not less than 93.12%.The water-oil partition coefficient of quercetin is 2.05.The enrichment factor of quercetin in water is higher than that in serum samples.When 2% methanol is added into serum samples,the enrichment factor of quercetin is 99.54,reaching the highest,which is equivalent to 63.8% of the 156.01 of quercetin in pure water.In conclusion,this method has a wide application prospect due to low cost,easy,and high sensitivity.
关键词
中空纤维膜液相微萃取
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槲皮素
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高效液相色谱
Key words
hollow fiber liquid phase micro-extraction
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quercetin
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high performance liquid chromatography
Author summay
宝贵荣(1976-),女,博士,副教授,研究方向为分析化学和蒙药分析,765633821@qq.com
HF-LPME与HPLC联用测定槲皮素LogD和富集倍数[J].
现代化工, 2021, 41(2): 265-269 DOI:10.16606/j.cnki.issn0253-4320.2021.02.050