基于漂浮有机液滴凝固液相微萃取的黄酮类化合物分配系数及含量测定

以漂浮有机液滴凝固液相微萃取（SFODLPME）对中药中黄酮类化合物进行富集，建立SFODLPME-HPLC快速测定中药材样品中低丰度黄酮类化学成分含量的方法. 并讨论了黄酮类化合物富集倍数与浓度之间的关系、富集倍数与供相体积之间的关系，定义和阐述了EF1μg?mL-1及其物理意义，计算了漂浮有机液滴凝固相体积及黄酮类化合物的表观分配系数. 在SFODLPME的优化条件下结合高效液相色谱测得8种黄酮类成分的线性范围均为0.01~10.00μg/ml；检测限在1.0~0.01ng/mL；精密度RSD<7.0%；药材中分析物的回收率在96.0% ~104.2%. 当加入萃取溶剂体积为40μl 时，形成漂浮有机液滴凝固相体积为52±14μl；8种黄酮类成分的表观分配系数在44.8~243.9之间.

Determination of Partition Coefficient and Contents of Flavonoids Compounds Based on Solidification of Floating Organic Drop Liquid-phase Microextraction

Flavonoids compounds were enriched by solidification of floating organic drop liquid-phase microextraction (SFODLPME). A method which rapidly determined the contents of low abundance flavonoids ingredients from traditional Chinese medicines(TCMs) samples by SFODLPME-HPLC was established. In this method, the relations between the enrichment factor and concentration of flavonoids compounds were revealed, EF1μg?mL-1 was defined and expounded; solidification phase volume of floating organic drop and apparent partition coefficient of flavonoids compounds were calculated by the relations between the enrichment factor and the donor phase volume of flavonoids compounds. Under the optimal conditions of SFODLPME, the linear ranges of eight kinds of flavonoids ingredients were 0.01~10.00μg/ml; the limits of detection (LODs) were 1.0~0.01ng/mL(S/N=3); the RSDs were less than 7.0%; the average recoveries of analytes in TCMs ranged from 96.0% to 104.2%. Solidification phase volume of floating organic drop was 52±14μl when extraction solvent volume is 40μl; Apparent partition coefficients of eight kinds of flavonoids ingredients ranged from 44.8 to 243.9.