Xu Jing-Jing, Cao Jun, Peng Li-Qing, Cao Wan, Zhu Qiong-Yao, Zhang Qian-Yun
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China.
College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou 310036, China.
J Chromatogr A. 2016 Mar 4;1436:64-72. doi: 10.1016/j.chroma.2016.01.046. Epub 2016 Jan 22.
Here, a novel β-cyclodextrin (β-CD) based trace matrix solid-phase dispersion (MSPD) method was developed to extract isomers from different honeysuckle samples using ultrahigh performance liquid chromatography. The structures of the analytes were characterized and determined via quadrupole time-of-flight tandem mass spectrometry and nuclear magnetic resonance. Under optimum conditions, 25mg of sample was dispersed with 75mg of β-CD, and 0.5mL of methanol was used as the elution solvent. The proposed method produced a good linearity (r(2)>0.99) for the isomers, with limits of detection ranging from 1.62 to 3.33ng/mL. The average recovery values that were obtained from analyzing the spiked samples were calculated to be in the range of 87.04-105.20%. Moreover, the trace MSPD method required less reagents and a shorter extraction time in comparison with the traditional pharmacopoeia method and other reported approaches. The developed method was successfully applied for the determination of three real honeysuckle samples that were collected from different cultivated areas.
在此,开发了一种基于新型β-环糊精(β-CD)的微量基质固相分散(MSPD)方法,用于使用超高效液相色谱从不同金银花样品中提取异构体。通过四极杆飞行时间串联质谱和核磁共振对分析物的结构进行了表征和测定。在最佳条件下,将25mg样品与75mgβ-CD分散,并用0.5mL甲醇作为洗脱溶剂。所提出的方法对异构体具有良好的线性(r(2)>0.99),检测限范围为1.62至3.33ng/mL。通过分析加标样品获得的平均回收率计算为87.04 - 105.20%。此外,与传统药典方法和其他报道的方法相比,微量MSPD方法所需试剂更少,提取时间更短。所开发的方法成功应用于测定从不同种植区采集的三个真实金银花样品。