Optimization of mechanically assisted coamorphous dispersion extraction of hydrophobic compounds from plant tea (Citri Reticulatae Pericarpium) using water.

This study aimed to establish a novel mechanically assisted coamorphous dispersion extraction (MADE) method for the extraction of hydrophobic compounds (hesperidin, nobiletin and tangeretin) from Citri Reticulatae Pericarpium using water. The surface morphology, particle size distributions, phase states and functional groups of the coground product surface were characterized by Scanning Electron Microscopy, X-ray diffraction and Fourier transform infrared spectroscopy. The parameters affecting the efficiency of extraction method were optimized by single-factor experiments and response surface methodology. The method showed good linear relationships in the range of 1-500 µg/mL with correlation coefficients (R2) ≥ 0.9990, low limits of detection ranging from 3.0 to 28.3 ng/mL, and acceptable recoveries ranging from 87.0 to 91.0%. Therefore, the proposed MADE method is a promising, efficient and organic solvent-free method for the extraction of hydrophobic compounds from plant tea.

The two-phase amphiphilic preconcentration based on surfactants to enrich phenolic compounds from diluted plant extracts and rat urine by micellar electrokinetic chromatography.

A novel technology by two-phase amphiphilic preconcentration based on surfactants was established for enriching phenolic compounds by micellar electrokinetic chromatography (MEKC). The cationic surfactant cetyltrimethylammonium chloride (CTAC) was combined with the anionic analytes that existed in the sample solution before injection. The boundary was formed between CTAC and sodium dodecyl sulfate (SDS) in the background solution when the sample solution was injected into the capillary, where the analytes bound inside micelles were released due to the stronger electrostatic force between SDS and CTAC. This procedure accelerated the separation of analytes from CTAC and greatly improved the enrichment efficiency. The optimal conditions were obtained after a series of optimizations, and the sensitivity enrichment factors of the four analytes were in the range of 39-93 compared to typical injections in capillary zone electrophoresis. Good linearity for matrix-matched calibrations was established for all analytes with R2 values of 0.9993-0.9997. The limits of detection (S/N = 3) for kaempferol, quercetin, salvianolic acid C, and salvianolic acid B were 0.0166, 0.0292, 0.0215, and 0.0195 µg/ml, respectively. The intracapillary RSDs of the analytes ranged from 0.8% to 1.3% for migration time and from 0.4% to 1.8% for peak areas. The developed method was successfully applied to the determination of phenolic compounds, the main compounds of Salvia miltiorrhiza Bge., and had been validated for the determination of spiked recoveries in rat urine.

Boron nitride nanosheet-assisted matrix solid-phase dispersion microextraction of alkaloids from lotus plumule by high-performance liquid chromatography coupled with ultraviolet detection and ion mobility quadrupole time-of-flight mass spectrometry.

A boron nitride nanosheet (BNNS)-assisted matrix solid-phase dispersion method was established to microextract alkaloids from medicinal plants. The target compounds were identified by high-performance liquid chromatography coupled with ultraviolet detection and ion mobility quadrupole time-of-flight mass spectrometry. During the experimental process, several important parameters, including the type of dispersant, the amount of dispersant, the grinding time, and the type of elution solvent, were optimized. Finally, the BNNSs were chosen as the best dispersant, and their microcosmic morphologies were identified by scanning electron microscopy and transmission electron microscopy. Because of the special property of BNNSs, the cost of this experiment was greatly reduced, especially in elution volume, sample amount (50 mg), and extraction time (2 min). Under the best conditions, 50 mg of sample powder was dispersed with 50 mg of BNNSs, the grinding time was 120 s, the mixed powder was eluted with 200 µL of methanol, and good linearity (r2  > 0.9993) and satisfactory recoveries (80-100%) were obtained. The inter- and intraday precisions were acceptable, with RSDs lower than 2.01 and 4.84%, respectively. The limits of detection ranged from 2.54 to 15.00 ng/mL, and the limits of quantitation were 8.47 to 50.00 ng/mL. The proposed method was successfully applied for the determination of liensinine, isoliensinine, and neferine in lotus plumule.