Fast, sustainable, and simultaneous analysis of water- and fat-soluble vitamins by the two-dimensional microcarbon fiber fractionation system hyphenated with MS detection.

BACKGROUND: Vitamins are micronutrients that are required for normal growth and development of living organisms. However, due to their various chemical properties (e.g., acid-base behavior, the presence of numerous forms) and fluctuating concentration levels within complex matrices, simultaneous analysis of multi-class vitamins, including their active forms, is a challenging task. The growing nutrient shortage in foods is concerning for food consumers, manufacturers, and quality control organizations. Hence, a simple, fast, and greener approach that can simultaneously analyze multi-class vitamins is required to aid food testing and clinical laboratories in evaluating vitamin content more rapidly and accurately. RESULTS: A green and rapid analytical method based on online two-dimensional microscale carbon fiber/activated carbon fiber fractionation-mass spectrometry (2DµCFs-MS) was developed and validated for simultaneous determination of vitamins (water- and fat-soluble vitamins and some analogs) in food supplements and fortified energy drinks. Vitamins have been successfully separated into three different fractions using the minimum toxic solvent (only 0.7 mL of organic solvent) in a single run within 6 min. The limit of detection (LOD) ranges from 0.1 to 10.4 ng/mL, and the limit of quantification (LOQ) ranges from 0.39 to 34.5 ng/mL. The method also showed adequate repeatability and intermediate precision, with RSD<10 % and R2 > 0.99 for most vitamins. The analytical method was evaluated in terms of greenness, with an analytical greenness (AGREE) score of 0.68. SIGNIFICANCE: The 2DµCFs-MS system was developed to separate and detect multi-class vitamins simultaneously, which can be used as a beneficial tool to investigate vitamin content for food labeling and determining the vitamins in biological fluids and other complex samples. The developed method can tackle the challenge of simultaneous and fast routine analysis of multi-class vitamins.

Specific fractionation of ginsenosides based on activated carbon fibers and online fast screening of ginseng extract by mass spectrometry.

Ginseng is beneficial in the prevention of many diseases and provides benefits for proper growth and development owing to the presence of various useful bioactive substances of diverse chemical heterogeneity (e.g., triterpenoid saponins, polysaccharides, volatile oils, and amino acids). As a result, understanding the therapeutic advantages of ginseng requires an in-depth compositional evaluation employing a simple and rapid analytical technique. In this work, three types of surface-activated carbon fibers (ACFs) were prepared by gas-phase oxidation, strong acid treatment, and Plasma treatment to obtain CO2-ACFs, acidified-ACFs, and plasma-ACFs, respectively. Three prepared ACFs were compared in terms of their physicochemical characterization (i.e., surface roughness and functional groups). A separation system was built using a column with modified ACFs, followed by mass spectrometry detection to investigate and determine substances of different polarities. Among the three columns, CO2-ACFs showed the optimum separation effect. 13 strong polar compounds (12 amino acids and1 oligosaccharide) and 15 lesser polar compounds (ginsenosides) were separated and identified successfully within 4 min in the ginseng sample. The data obtained by CO2-ACFs-TOF-MS/MS and UHPLC-TOF-MS/MS were compared. Our approach was found to be faster (4 min vs. 36 min) and greener, requiring much less solvent (1 mL vs. 10.8 mL), and power (0.06 vs. 0.6 kWh). The developed methodology can provide a faster, eco-friendly, and more reliable tool for the high-throughput screening of complex natural matrices and the simultaneous evaluation of several compounds in diverse samples.

On the use of a 2D-carbon microfiber fractionation system to improve flow-injection QTOF-HRMS analysis in complex matrices: the case of Abelmoschus manihot flower extracts.

A two-dimensional microscale carbon fiber/active carbon fiber system combined with a quadrupole time of flight high-resolution mass spectrometry (2DµCFs-QTOF-HRMS) system is proposed for the rapid putative identification of polar, medium-polar and weakly polar constituents in complex matrices while strongly mitigating ionic suppression effects. The capabilities of 2DµCFs-QTOF-HRMS have been proven by analysing the composition of Abelmoschus manihot flower extracts, allowing, in a single run, the detection of 41 known substances and the presence of 6 compounds never revealed before in these samples. 2DµCFs-QTOF-HRMS has been compared with traditional HPLC-MS, showing higher versatility and a significant reduction of both analysis time (70 min to 5 min) and solvent consumption (35 mL to 1.5 mL). A comparison with the results obtained by direct flow-injection MS analyses demonstrated that 2DµCFs-QTOF-HRMS leads to a more comprehensive analysis and to improved detection sensitivity. The proposed method can be considered suitable for the rapid and comprehensive analysis of food, environmental and pharmaceutical complex samples. 2DµCFs-QTOF-HRMS can thus be considered a rapid, versatile, reliable, high-throughput and economical technique that allows for the collection of information on polar, semipolar, and weakly polar components in complex matrices.

Anesthetic constituents of Zanthoxylum bungeanum Maxim.: A pharmacokinetic study.

A sensitive and selective ultra high performance liquid chromatography with tandem mass spectrometry method was established and validated for the simultaneous determination of hydroxy-α-sanshool, hydroxy-ß-sanshool, and hydroxy-γ-sanshool in rat plasma after the subcutaneous and intravenous administration of an extract of the pericarp of Zanthoxylum bungeanum Maxim. Piperine was used as the internal standard. The analytes were extracted from rat plasma by liquid-liquid extraction with ethyl acetate and separated on a Thermo Hypersil GOLD C18 column (2.1 mm × 50 mm, 1.9 µm) with a gradient elution system at a flow rate of 0.4 mL/min. The mobile phase consisted of acetonitrile/0.05% formic acid in water and the total analysis time was 4 min. Positive electrospray ionization was performed using multiple reaction monitoring mode for the analytes. The calibration curves of the three analytes were linear over the tested concentration range. The intra- and interday precision was no more than 13.6%. Extraction recovery, matrix effect, and stability were satisfactory in rat plasma. The developed and validated method was suitable for the quantification of hydroxy-α-sanshool, hydroxy-ß-sanshool, and hydroxy-γ-sanshool and successfully applied to a pharmacokinetic study of these analytes after subcutaneous and intravenous administration to rats.