超分子有序聚集凝固液相微萃取及其对五味子中木脂素类化合物的测定及质量评价

通过分析比较漂浮有机液滴凝固液相微萃取(SFODLPME)对木脂素类化合物萃取前后紫外光谱的变化, 提出了超分子有序聚集凝固液相微萃取(SSMOALPME)机理; 建立了简单、 快速、 灵敏的SSMOALPME高效液相色谱法(HPLC)同时测定中药五味子中5种低丰度木脂素类化合物含量的方法, 并对不同产地五味子的质量进行比较和评价. 在最佳的SSMOALPME条件下, 测得五味子醇甲, 五味子酯甲, 五味子甲素, 五味子乙素和五味子丙素的线性范围分别为2.48×10^-3~6.21, 2.27×10^-3~28.5, 2.31×10^-3~28.8, 2.27×10^-3~5.69和1.05×10^-3~5.25 μg/mL; 检出限分别为0.4, 0.4, 0.4, 0.08和0.08 ng/mL; 日内及日间精密度RSD<9.7%; 药材中分析物的回收率为91.9% ~104.7%; SSMOALPME对5种分析物的富集倍数分别在39 ~529倍之间. 本法测定结果与药典法测定结果相比无显著差异(P=95%). SSMOALPME方法的提出为液相微萃取的理论研究奠定了基础, 为反映中药多成分、 多靶点及协同作用的特性, 建立科学的质量控制方法提供了理论依据和实验基础.

Solidification of Superamolecule Ordering Assembly Liquid Phase Microextraction and Its Application for the Determination and Evaluation for Lignans Quality in Schisandra Chinensis( Turcz.) Baill

The extraction mechanism of solidification of superamolecule ordering assembly liquid phase microextraction(SSMOALPME) was proposed based on the change in the UV spectra of lignan compounds before and after the solidification of floating organic drop liquid phase microextraction(SFODLPME).SSMOALPME coupled with high performance liquid chromatography(HPLC) was introduced for the determination and eva-luation of five low abundance lignan compounds in Schisandra chinensis(Turcz.) Baill from different origins.Under the optimized parameters,the linear ranges of schisandrol A,schisantherin A,schizandrin A,schizandrin B and schizandrin C were 2.48×10-3—6.21,2.27×10-3—28.5,2.31×10-3—28.8,2.27×10-3—5.69 and 1.05×10-3—5.25 μg/mL,the limits of detection(LODs) were 0.4,0.4,0.4,0.08 and 0.08 ng/mL,respectively,the intra and inter RSDs were less than 9.7%,the mean recoveries of analytes in traditional Chinese medicines(TCMs) were between 91.9% and 104.7%,and the enrichment factors(EFs) were in the range of 39—529 for SFODLPME.There was no significant difference in results determined lignan compounds in Schisandra chinensis(Turcz.) Baill by this method and Pharmacopoeia method(P=95%).SSMOALPME-HPLC provide the theoretic foundation and experimental evidence for reflecting bioactive component characteristics of multicomponent,multi-targets,synergistic effect,and establishing scientific quality control methods in TCMs.