Ultrasonic Solvent Extraction Followed by Dispersive Solid Phase Extraction (d-SPE) Cleanup for the Simultaneous Determination of Five Anthraquinones in Polygonum multiflorum by UHPLC-PDA

Abstract

A rapid and effective ultra-high performance liquid chromatography (UHPLC) method was developed for the determination of five anthraquinones (emodin, physcion, aloe-emodin, rhein, and chrysophanol) in Polygonum multiflorum. The target compounds were ultrasonically extracted with 70% methanol, followed by dispersive solid-phase extraction (d-SPE) with HC-C18 and desorption with acetonitrile. The five anthraquinones were separated on an ACQUITY UPLC ® HSS T3 column (2.1 × 100 mm, 1.8 μm) and detected by a photodiode array detector (PDA) at 254 nm. Under the optimized conditions, linear relationships were achieved in the range of 0.3~100 mg/L for emodin, 0.3~40 mg/L for physcion, 0.1~20 mg/L for aloe-emodin, and 0.05~20 mg/L for rhein and chrysophanol. The limits of detection of the five analytes ranged from 0.01 to 0.08 mg/L, and the recoveries were within the range of 82.8~118.4% with an RSD (n = 6) of 1.0~10.3%. The intra-day and inter-day precision (n = 5) of the five targets were in the range of 1.0~1.8% and 3.0~3.1%, respectively. Furthermore, this method was applied to analyses of Polygonum multiflorum samples collected from different regions in China with satisfactory results. All the results indicated that this method is suitable for the detection of five anthraquinones in Polygonum multiflorum.

Simultaneous Electrochemical Detection of Cd2+ and Pb2+ Based on an MOF-Derived Carbon Composite Linked with Multiwalled Carbon Nanotubes

“…MOF materials have attracted extensive attention in the field of electrocatalysis due to their high specific surface area, tunable pore size, diversity of central metals, organic ligands, and easy structure tunability . Among them, zeolitic imidazolate frameworks (ZIFs) have become a well-known family of MOFs due to their zeolite-like structure, demonstrating broad application potential in energy storage, adsorption, catalysis, gas separation, supercapacitors, batteries, and electrochemical sensors . However, the poor electrical conductivity of most MOFs restricts the transfer paths of electrons, which also limits the electron transfer paths on the electrode surface.…”

Magnetic porous carbon derived from NH2‐MIL‐101(Fe) as an adsorbent for the magnetic solid‐phase extraction of anthraquinones

“…The analytical performance of the developed NH 2 ‐MIL‐101‐C‐based MSPE‐HPLC method was compared with some previously reported methods for AQs determination [37–40]. As summarized in Table 1, the current method has comparable linearity, good precision, and adequately low detection limits.…”

Ultrasound-assisted extraction of emodin from Rheum officinale Baill and its antibacterial mechanism against Streptococcus suis based on CcpA

“…Subsequently, 0.5 g of fruit powder was fully mixed with a certain amount of solution, and the mixture was placed in an ultrasonic homogenizer (JY92-2D, Xinzhi Bio-Sciences Co. Ltd., Ningbo, China) with a frequency of 20 kHz at 25 °C. By consulting literature, three liquids (water, methanol and ethanol aqueous solutions (83 %, v / v ) were selected as extraction solvents, and the suitable extraction solvent was determined through the comparison of yield, dynamic simulation analysis and scanning electron microscope (SEM) observation [35] , [36] , [37] , [38] . The effects of ultrasound treatment on the R. officinale powders were observed on a scanning electron microscope (SU8010, Hitachi, Japan).…”