Abstract

In this study, matrix solid phase dispersion (MSPD) microextraction combined with supercritical fluid chromatography-ion mobility quadrupole time-of-flight mass spectrometry (SFC/IM-QTOF-MS) was used to analyze the multipolar compounds in plant tea. The parameters of stationary phase, mobile phase, make-up solution, temperature, and back pressure were optimized. The target analytes were gradient eluted in 8 min by supercritical CO2 on a Zorbax RX-SIL column. Collisional Cross Section (CCS) values for single and multiple fields were measured. A series of validation studies were carried out under the optimal conditions, and the linear relationship and reproducibility were good. The limits of detection were 1.4 (Scoparone (1))~70 (Naringenin (4)) ng/mL, and the limits of quantification were 4.7 (Scoparone (1))~241 (Naringenin (4)) ng/mL. The recoveries of most compounds ranged from 60.7% to 127%. As a consequence, the proposed method was used for the separation and quantitative analysis of active ingredients in caulis dendrobii.

Highlights

  • Supercritical fluid chromatography (SFC) is generally is a chromatography technique in which the mobile phase is supercritical carbon dioxide (SCCO2) or subcritical carbon dioxide [1]

  • CO2 was used in mobile phase A, methanol was used in mobile phase B, and 0.1% acetic acid was used in the make-up solution

  • The reason for the short retention time may be that the polarity of the stationary phase was too large, which resulted in the co-elution of the tested compound

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Summary

Introduction

Supercritical fluid chromatography (SFC) is generally is a chromatography technique in which the mobile phase is supercritical carbon dioxide (SCCO2) or subcritical carbon dioxide [1] These fluids are close to or surpass critical temperature and/or pressure of CO2, and have the advantage of low viscosity and high diffusivity, enabling rapid analysis of target compounds with high resolution [2]. Gao et al isolated six flavonoid aglycones by using Poroshell 120 EC-CN as a chromatographic column and adding 20 mM [Bmim] [BF4] as a mobile phase modifier in SFC [7]. Most of these studies only covered flavonoids widely present in traditional Chinese medicine and could not analyze compounds with different structures at the same time. It makes sense to further expand the application of SFC

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