A Diol-Based-Matrix Solid-Phase Dispersion Method for the Simultaneous Extraction and Determination of 13 Compounds From Angelicae Pubescentis Radix by Ultra High-Performance Liquid Chromatography

METHODS published: 08 March 2019 doi: 10.3389/fphar.2019.00227 A Diol-Based-Matrix Solid-Phase Dispersion Method for the Simultaneous Extraction and Determination of 13 Compounds From Angelicae Pubescentis Radix by Ultra High-Performance Liquid Chromatography Edited by: Lillian Barros, Polytechnic Institute of Bragança, Portugal Reviewed by: Jun Cao, Hangzhou Normal University, China Dejan S. Stojkovic, University of Belgrade, Serbia *Correspondence: Yan-xu Chang ; † These authors have contributed equally to this work and share first authorship Specialty section: This article was submitted to Ethnopharmacology, a section of the journal Frontiers in Pharmacology Received: 24 December 2018 Accepted: 22 February 2019 Published: 08 March 2019 Citation: Ding M, Bai Y, Li J, Yang X, Wang H, Gao X and Chang Y-x (2019) A Diol-Based-Matrix Solid-Phase Dispersion Method for the Simultaneous Extraction and Determination of 13 Compounds From Angelicae Pubescentis Radix by Ultra High-Performance Liquid Chromatography. Front. Pharmacol. 10:227. doi: 10.3389/fphar.2019.00227 Mingya Ding 1,2† , Yun Bai 1,2† , Jin Li 1,2 , Xuejing Yang 3 , Hui Wang 1,2 , Xiumei Gao 1,2 and Yan-xu Chang 1,2* 1 Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin, China, Tianjin Key Laboratory of Phytochemistry and Pharmaceutical Analysis, Tianjin University of Traditional Chinese Medicine, Tianjin, China, 3 School of Pharmacy, Harbin University of Commerce, Harbin, China 2 A simple and eco-friendly Diol-based-matrix solid-phase dispersion method (MSPD) was optimized and established to simultaneously extract 13 bioactive compounds (7 coumarins and 6 phenolic acids) in Angelicae Pubescentis Radix (APR) by ultrahigh performance liquid chromatography coupled with photodiode array detector (UHPLC-PDA). Diol was chosen as the dispersing sorbent and methanol solution was used as the elution solvent. The preparation procedures for the MSPD including the types of sorbents, mass ratio of matrix to sorbent, grinding time, type, concentration and volume of elution solvent were investigated. Under the optimal conditions, good recoveries of the 13 target compounds were obtained in the range of 94.8–107% (RSD < 3.22%). The limits of detection (LODs) and limits of quantitation (LOQs) were in the ranges of 0.08–0.12 µg mL−1 and 0.16–0.24 µg mL−1 , respectively. Compared with the traditional method, it was a green and environmentally friendly technique. The results proved that the established method was successfully applied to the extraction and determination of 13 target bioactive compounds for quality control in APR. Keywords: Angelicae Pubescentis Radix, coumarins, Diol-matrix solid-phase dispersion, phenolic acids, UHPLC INTRODUCTION Angelicae Pubescentis Radix (APR), the dried roots of Angelica pubescens Maxim, f. biserrata Shan et Yuan, belonged to the Apiaceae family. It was named as Duhuo in Chinese as a commonly used traditional Chinese medicine (TCM) (Chinese Pharmacopoeia Commission, 2015). It was first recorded in Shennong’s Classic of Materia Medica and medically used during the NorthSouth Dynasty period (Cao and Li, 2018). APR is wildly used to treat rheumatic disease in the Frontiers in Pharmacology | www.frontiersin.org 1 March 2019 | Volume 10 | Article 227 Ding et al. A Diol-Based-MSPD Method for the Extraction Compounds From APR method for the simultaneous extraction of 6 phenolic acids (neochlorogenic acid, chlorogenic acid, 4-dicaffeoylquinic acid, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C) and 7 coumarins (umbelliferae, columbianetin, columbianetin acetate, imperatorin, osthole, isoimperatorin, and columbianadin) in APR by ultrahigh performance liquid chromatography coupled with PDA detection (UHPLC-PDA). The Diol was firstly employed to extract multiple components of APR during the MSPD procedure. The potential influential parameters such as the types of sorbents, mass ratio of matrix to sorbent, grinding time, eluent type, concentration and volume of eluent were investigated for acquiring optimal extraction efficiency. clinics in China (Wang et al., 2008). Recently, many studies have revealed that APR has the anti-tumor, anti-inflammation, antiproliferatory, anti-platelet aggregation and anthelmintic activities (Liu et al., 1998, 2010; Wang et al., 2010; Chang et al., 2013). The chemistry compositions of APR included coumarins, phenolic acids, essential oils, organic acids, and saccharides (Chen, 2014). It was reported that coumarins were the most abundant in APR (Chang et al., 2011). The coumarins have attracted extensive attention worldwide. However, other compounds covering phenolic acids also have a series of pharmacological activities such as anti-oxidant and immune regulation. Moreover, osthole and columbianadin were the quality control markers in Chinese Pharmacopoeia Commission (2015 Version), which may not be specific and meaningful (Chinese Pharmacopoeia Commission, 2015). Therefore, the complete extraction and precise analysis of coumarin and phenolic acid compounds are particularly important for quality control and physiological and pharmacological investigations. Currently, many analytical methods for determining multiple components in APR have been developed by high-performance liquid chromatography with diode array detector (HPLC-DAD), gas chromatography-mass spectrometry (GC-MS), and highperformance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-Q-TOF/MS) (Yang et al., 2006; Ge et al., 2014; Zhang et al., 2017; Wang J. R. et al., 2018). The commonly used extraction method of APR is ultrasonic-assisted extraction (UAE), which not only need large amounts of samples and a great deal of organic solvents, but also need much extraction times. Matrix solid phase dispersion (MSPD) as a promising sample extraction technique was normally employed to extract the solid, semisolid, and highly viscous biological samples by disrupting and dispersing the solid sorbent in the sample (Barker et al., 1989; Liu et al., 2008; VelaSoria et al., 2014; Li et al., 2017). Its unique properties is that integrating sample matrix disruption, extraction, fractionation and clean up in one single process could reduce the consumption of organic solvents and deliver cost savings (Barker et al., 1989). To our knowledge, no literatures have been reported on MSPD as an extraction method for the simultaneous extraction of coumarins and phenolic acids in APR. It has been reported that the selection of a suitable sorbent was one of the vital procedures in the development of the MSPD (Enríquez-Gabeiras et al., 2012). The sorbent could be used to disrupt the sample architecture, and employed to disperse analytes onto a solid phase support to generate powerful sample-solvent interactions (Wang H. L. et al., 2018). The commonly sorbent in MSPD were reversed-phase material [C18 (...truncated)