Two-step pressure injection-assisted online enrichment of herbicides from foods with affinity micelle sweeping by micellar electrokinetic chromatography.

A novel online two-step pressure injection-assisted stacking preconcentration method, which involves sweeping and affinity micelles in micellar electrokinetic chromatography was developed to simultaneously measure various organic anions. The micellar solution was a mixed solution that contained 0.3 mM didodecyldimethylammonium bromide and 20 mM borax. After the micellar solution was injected for 60 s, the tested analytes prepared in 20 mM borax were introduced into the capillary for 150 s. The key experimental factors that influenced the separation and sensitivity were investigated and optimized, including the concentration and injection time of the micellar solution, the concentration of borax in the sample solution, the concentration of sodium dodecyl sulfate and borax in the background electrolyte (BGE), the content of acetonitrile in the BGE and the injection time of the sample solution. Compared with typical injection methods, this method achieved sensitivity enhancement factors ranging from 85 to 97 under optimized conditions. Good linearity for matrix-matched calibration was established for all analytes with R2 values of 0.9986-0.9996. The intraday (n = 6) and interday (n = 6) precisions of the method were less than 2.85% when expressed as relative standard deviations. When the method was applied to analyze rice and dried ginger samples, analyte recoveries ranged from 85.81% to 106.59%. Through sweeping and affinity micelles, stacking preconcentration method was successfully employed to analyze trace amounts of fenoprop and 2,4-dichlorophenoxyacetic acid in rice and dried ginger samples.

Enzyme activity- and chemometrics-assisted comprehensive two-dimensional liquid chromatography coupled with ion mobility quadrupole time-of-flight mass spectrometry for the analysis of honeysuckle.

A unique and effective comprehensive two-dimensional liquid chromatography system was established and applied for the analysis of bioactive components in honeysuckle. Under the optimal conditions, Eclipse Plus C18 (2.1 × 100 mm, 3.5 µm, Agilent) and SB-C18 (4.6 × 50 mm, 1.8 µm, Agilent) columns were chosen for the first dimension (1D) and the second dimension (2D) separation. The optimal flow rates of 1D and 2D were 0.12 mL/min and 2.0 mL/min, respectively. Additionally, the proportion of organic solution was optimized to enhance orthogonality and integrated shift, and full gradient elution mode was adopted to improve chromatographic resolution. Furthermore, a total of 57 compounds were identified by molecular weight, retention time and collision cross-section value obtained from ion mobility mass spectrometry. Based on the data obtained from the principal component analysis, partial least squares discriminant analysis, and hierarchical cluster analysis, the categories of honeysuckle in different regions were significantly different. Moreover, the half maximal inhibitory concentration values of most samples were between 0.37 and 1.55 mg/mL, and most samples were potent α-glucosidase inhibitors, which is better for the evaluation of the quality of drugs from two aspects of substance content and activity.