Microwave-assisted extraction followed by salting-out phase separation for hierarchical screening of illegal adulterants in aphrodisiac health products by multi-dimensional fingerprint profiling analysis

Abstract

A novel method for hierarchical screening of illegal adulterants in Fur seal ginseng pills (FSGP) products was developed by microwave-assisted extraction (MAE) coupled to salting-out assisted liquid-liquid extraction (SALLE) with multi-dimensional fingerprint profiling analysis. Using a homogeneous system formed by dimethyl carbonate (DMC) and water as the extractant, the MAE conditions were investigated to maximize extraction recoveries, followed by addition of ammonium sulfate to induce DMC phase separation for SALLE enrichment of 16 potentially illegal adulterants such as phosphodiesterase type-5 inhibitors, androgens, α receptor antagonists and yohimbine etc. By means of high-performance liquid chromatography (HPLC) with diode array detection (DAD) and fluorescence detection (FLD), multi-dimensional fingerprints were acquired by multi-wavelength detection to highlight the signals of the potentially illegal adulterants and reduce or remove interferences from the sample matrix. For high accuracy and reliability, a hierarchical screening strategy was designed by multi-dimensional fingerprinting profiling analysis (MDFPA). The method exhibited proper identification and quantification performance, and it was successfully applied to screening of illegal adulterants in 18 batches of the samples through the step-by-step MDFPA. Also, the results were further confirmed by ultra high-performance liquid chromatography-quadrupole-orbitrap mass spectrometry (UHPLC-Q-Orbitrap/MS). The proposed method was proved to be a green, efficient and reliable alternative to monitoring aphrodisiac health products.