Du Kunze, Li Jin, Tian Fei, Chang Yan-Xu
Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin, 300193, China; Key Laboratory of Formula of Traditional Chinese Medicine (Tianjin University of Traditional Chinese Medicine), Ministry of Education, Tianjin, 300193, China.
Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin, 300193, China; Key Laboratory of Formula of Traditional Chinese Medicine (Tianjin University of Traditional Chinese Medicine), Ministry of Education, Tianjin, 300193, China.
J Pharm Biomed Anal. 2018 Feb 20;150:59-66. doi: 10.1016/j.jpba.2017.12.003. Epub 2017 Dec 5.
A simple nonionic detergent - based vortex- synchronized matrix solid-phase dispersion (ND-VSMSPD) method was developed to extract bioactive compounds in Forsythiae Fructus coupled with ultra high-performance liquid chromatography (UHPLC). Nonionic detergent Triton 114 was firstly used as a green elution reagent in vortex- synchronized MSPD procedure. The optimum parameters were investigated to attain the best results, including Florisil as sorbent, 2mL 10% (v/v) nonionic detergent Triton X-114 as the elution reagent, 1:1 of sample/sorbent ratio, grinding for 3min, and whirling for 2min. The recoveries of the six compounds in Forsythiae Fructus were in the range of 95-104% (RSD <4.6%) and the method displayed a good linearity within the range of 0.08-20μgmL for caffeic acid, 0.6-150μgmL for forsythoside A, 0.4-100μgmL phillyrin, 0.2-50μgmL for quercetin, isorhamnetin and arctigenin (r≥0.999). It was proved that the extraction yields of almost all compounds attained by the established vortex- synchronized MSPD, which required lower sample, reagent and time, were higher than the normal MSPD and the traditional ultrasonic-assisted extraction. Consequently, this developed vortex- synchronized MSPD coupled with simple UHPLC method could be efficiently applies to extract and analyze the target compounds in real Forsythiae Fructus samples.
建立了一种基于简单非离子型洗涤剂的涡旋同步基质固相分散法(ND-VSMSPD),用于提取连翘中的生物活性成分,并结合超高效液相色谱(UHPLC)进行分析。非离子型洗涤剂吐温114首次在涡旋同步基质固相分散法中用作绿色洗脱剂。研究了最佳参数以获得最佳结果,包括使用弗罗里硅土作为吸附剂,2mL 10%(v/v)非离子型洗涤剂吐温X-114作为洗脱剂,样品/吸附剂比例为1:1,研磨3分钟,涡旋2分钟。连翘中六种化合物的回收率在95-104%范围内(相对标准偏差<4.6%),该方法在0.08-20μg/mL的咖啡酸、0.6-150μg/mL的连翘苷A、0.4-100μg/mL的连翘酯苷、0.2-50μg/mL的槲皮素、异鼠李素和牛蒡子苷元范围内呈现良好的线性关系(r≥0.999)。结果表明,所建立的涡旋同步基质固相分散法所需样品、试剂和时间较少,几乎所有化合物的提取率均高于常规基质固相分散法和传统超声辅助提取法。因此,这种改进的涡旋同步基质固相分散法结合简单的UHPLC方法可有效地应用于实际连翘样品中目标化合物的提取和分析。