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

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

利用漂浮有机液滴凝固液相微萃取（SFODLPME）技术对中药中的黄酮类化合物进行富集,建立了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.讨论了黄酮类化合物的富集倍数与浓度及与供相体积之间的关系,定义并阐述了富集倍数（EF1μg/mL）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.在优化的SFODLPME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;检出限为1.0~0.01 ng/mL;精密度RSD〈7.0%;药材中分析物的回收率为96.0%~104.2%.当加入的萃取溶剂体积为40μL时,形成的漂浮有机液滴凝固相体积为（52±14）μL;8种黄酮类成分的表观分配系数在44.8~243.9之间.

Flavonoids compounds were enriched by solidification of floating organic drop liquid-phase microextraction（SFODLPME）.A rapid determination method for 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（EF） and the concentration of flavonoids compounds were revealed,EF1 μg/mL 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_10.00 μg/mL;the limits of detection（LODs） were {1.0_0.01} ng/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±14） μL when extraction solvent volume is 40 μL;apparent partition coefficients of eight kinds of flavonoids ingredients ranged from 44.8 to 243.9.