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基于微晶纤维素的基质固相分散微萃取结合超高效液相色谱-四极杆飞行时间质谱法测定枇杷叶中异构三萜酸

Microcrystalline cellulose based matrix solid phase dispersion microextration for isomeric triterpenoid acids in loquat leaves by ultrahigh-performance liquid chromatography and quadrupole time-of-flight mass spectrometry.

作者信息

Cao Jun, Peng Li-Qing, Xu Jing-Jing

机构信息

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.

出版信息

J Chromatogr A. 2016 Nov 11;1472:16-26. doi: 10.1016/j.chroma.2016.10.034. Epub 2016 Oct 13.

Abstract

An analytical procedure based on matrix solid phase dispersion (MSPD) microextration and ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry was developed for the determination of isomeric triterpenoid acids (maslinic acid, corosolic acid, oleanolic acid and ursolic acid) in loquat leaves. Microcrystalline cellulose was used for the first time as a solid sorbent in MSPD microextration. Compared with the traditional extraction methods, the proposed method possessed the advantages of shorter extraction time, and lower consumption of sample, sorbent and organic solvent. The MSPD parameters that influenced the extraction efficiency of isomeric analytes were investigated and optimized in detail. Under the optimized conditions, good linearity was obtained with correlation coefficients higher than 0.9990. The limits of detection and quantification were 19.6-51.6μg/kg and 65.3-171.8μg/kg, respectively. Meanwhile, the recoveries obtained for all the analytes were ranging from 90.1% to 107.5%. Finally, the optimized method was successfully applied for analyzing these isomeric acids in loquat leaves samples obtained from different cultivated areas.

摘要

建立了一种基于基质固相分散(MSPD)微萃取和超高效液相色谱-四极杆飞行时间串联质谱联用的分析方法,用于测定枇杷叶中异构三萜酸(山楂酸、科罗索酸、齐墩果酸和熊果酸)的含量。微晶纤维素首次被用作MSPD微萃取中的固体吸附剂。与传统萃取方法相比,该方法具有萃取时间短、样品、吸附剂和有机溶剂消耗低等优点。详细研究并优化了影响异构分析物萃取效率的MSPD参数。在优化条件下,获得了良好的线性关系,相关系数高于0.9990。检测限和定量限分别为19.6 - 51.6μg/kg和65.3 - 171.8μg/kg。同时,所有分析物的回收率在90.1%至107.5%之间。最后,该优化方法成功应用于分析来自不同种植区域的枇杷叶样品中的这些异构酸。

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