Abstract

Practicing “green analytical chemistry” is of great importance when profiling the chemical composition of complex matrices. Herein, a novel hybrid analytical platform was developed for direct chemical analysis of complex matrices by online hyphenating pressurized warm water extraction followed by turbulent flow chromatography coupled with high performance liquid chromatography-tandem mass spectrometry (PWWE-TFC-LC-MS/MS). Two parallel hollow guard columns acted as extraction vessels connected to a long narrow polyether ether ketone tube, while warm water served as extraction solvent and was delivered at a flow rate of 2.5 mL/min to generate considerable back pressure at either vessel. A column oven heated both the solvent and crude materials. A TFC column, which is advantageous for the comprehensive trapping of small molecular substances from fluids under turbulent flow conditions, was employed to transfer analytes from the PWWE module to LC-MS/MS. Two electronic valves alternated each vessel between extraction and elution phases. As a proof-of-concept, a famous herbal medicine for the treatment of neurodegenerative disorders, namely Polygalae Radix, was selected for the qualitative and quantitative analyses. The results suggest that the hybrid platform is advantageous in terms of decreasing time, material, and solvent consumption and in its automation, versatility, and environmental friendliness.

Highlights

  • Capability of water into the sample matrix and mass transfer rates of the compounds from the plant tissue matrix, which improves the extraction efficiency[11]

  • Higher responses for the peaks that eluted before 10 min are shown in Fig. S1A compared with Fig. S1B,D, whereas comparable responses are observed for the peaks that eluted after 10 min among Fig. S1A,B and D

  • Comparable responses are shown for the peaks that eluted before 10 min in Fig. S1A,C, whereas Fig. S1A shows higher responses for the components that eluted after 10 min than those in Fig. S1C, which suggests that the pressurized warm water extraction (PWWE) module provided a greater extraction efficiency than sonication with pure water, in particular for the less polar compounds

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Summary

Introduction

Capability of water into the sample matrix and mass transfer rates of the compounds from the plant tissue matrix, which improves the extraction efficiency[11]. A high solvent flow-rate is beneficial to PLE for extracting crude materials, it creates challenges for the extraction efficiency of the SPE column. This requirement fits well with the principle of turbulent flow chromatography (TFC), which is a special SPE technique that is useful for the comprehensive extraction of small molecular weight components from fluids under turbulent flow conditions inside a TFC column. As a proof of concept, Polygalae Radix, the dried roots of Polygala tenuifolia Willd, which is one of the most widely used traditional Chinese medicines and plays an important role for improving the ecological environments of the Loess Plateau in China, was employed as a case study to validate the applicability of online PWWE-TFC-LC-MS/MS. This famous herbal medicine has been demonstrated as a promising candidate for the treatment of neurodegenerative disorders, e.g., Alzheimer’s disease (AD)[16,17]

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