College of Chemistry and Life Science, Changchun University of Technology, Changchun, 130012, PR China.
College of Chemistry and Life Science, Changchun University of Technology, Changchun, 130012, PR China; College of Chemistry, Jilin University, Changchun, 130012, PR China.
J Pharm Biomed Anal. 2019 Jan 30;163:95-104. doi: 10.1016/j.jpba.2018.09.050. Epub 2018 Sep 28.
Ionic liquid-based salt-induced liquid-liquid extraction was developed for the first time and applied to the extraction of four active constituents, including polydatin, resveratrol, emodin, and physcion in Polygonum cuspidatum (P. cuspidatum). In this study, ionic liquid was used as extraction solvent. The dried P. cuspidatum samples purchased from the pharmacy were triturated and passed through a 120-mesh sieve. The obtained sample powders were dried to constant weight at 55 ℃, and then mixed with extraction solvent. The extraction was carried out with the aid of ultrasound. Three phases, including ionic liquid-rich, salt-rich and solid sample phases were formed in the presence of salt. The target analytes were enriched in ionic liquid phase and then determined by high performance liquid chromatography. The experimental parameters, such as type and volume of ionic liquid, type and amount of salt, pH value of extraction medium, ultrasound power, ultrasound time and centrifugal condition, were optimized. The calibration curves showed good linear relationship (r > 0.9994). The limits of detection and quantification were in the range of 2.8-29.5 and 9.4-98.3 ng mL, respectively. The spiked recoveries were between 92.16% and 105.41%. Compared with hot reflux extraction and ultrasound-assisted extraction, the proposed method requires less extraction solvent and time. The present method can be applied to the determination of polyphenols and anthraquinones in P. cuspidatum.
离子液体盐辅助的液-液萃取法首次被开发出来，并应用于提取虎杖中的四种活性成分，包括白藜芦醇、大黄素、大黄素甲醚和虎杖苷。在本研究中，离子液体被用作萃取溶剂。从药店购买的干燥虎杖样品经研磨后通过 120 目筛。所得样品粉末在 55℃下干燥至恒重，然后与萃取溶剂混合。萃取在盐的存在下进行超声辅助。在盐的存在下形成了离子液体相、盐富相和固体样品相三相。目标分析物富集在离子液体相中，然后通过高效液相色谱法进行测定。实验参数，如离子液体的类型和体积、盐的类型和用量、萃取介质的 pH 值、超声功率、超声时间和离心条件等进行了优化。校准曲线呈现出良好的线性关系（r > 0.9994）。检测限和定量限范围分别为 2.8-29.5 和 9.4-98.3ng/mL。加标回收率在 92.16%至 105.41%之间。与热回流萃取和超声辅助萃取相比，该方法所需的萃取溶剂和时间更少。该方法可用于测定虎杖中的多酚和蒽醌类化合物。
