Simultaneous determination of 13 carbohydrates using high‐performance anion‐exchange chromatography coupled with pulsed amperometric detection and mass spectrometry

Abstract

A simple, accurate, and highly sensitive method was developed for the determination of 13 carbohydrates in polysaccharide of Spirulina platensis based on high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry. Samples were extracted with deionized water using ultrasonic-assisted extraction, and the ultrasound-assisted extraction conditions were optimized by Box-Behnken design. Then the extracted polysaccharide was hydrolyzed by adding 1 mol/L trifluoroacetic acid before determination by high-performance anion-exchange chromatography coupled with pulsed amperometric detection and confirmed by high-performance anion-exchange chromatography coupled with mass spectrometry. The high-performance anion-exchange chromatography coupled with pulsed amperometric detection method was performed on a CarboPac PA20 column by gradient elution using deionized water, 0.1 mol/L sodium hydroxide solution, and 0.4 mol/L sodium acetate solution. Excellent linearity was observed in the range of 0.05-10 mg/L. The average recoveries ranged from 80.7 to 121.7%. The limits of detection and limits of quantification for 13 carbohydrates were 0.02-0.10 and 0.2-1.2 μg/kg, respectively. The developed method has been successfully applied to ambient samples, and the results indicated that high-performance anion-exchange chromatography coupled with pulsed amperometric detection and mass spectrometry could provide a rapid and accurate method for the simultaneous determination of carbohydrates.

Green Synthesis of Gold Nanoparticles Using Carrageenan Oligosaccharide and Their In Vitro Antitumor Activity

“…The average absorbance of three parallel validation experiments at 530 nm was 1.295, which was well matched with the predicted value with a relative error of 7.48%, indicating that the model was suitable for synthetic condition optimization of CAO-AuNPs [21,27]. …”

“…Additionally, the “Adeq Precision” of 9.685 in our experiment indicated that the model with an adequate signal was suitable for the optimal design of this experiment. This RSM model was confirmed to fit the experimental optimization of synthesis of AuNPs well [21,22,27]. The 3D profiles and contour plots of multiple non-linear regression models (Figure S3) were depicted as a graphical interpretation of the experimental levels of each independent variable.…”

“…The quadratic regression model F -value of 11.94 with a low probability p -value (<0.05) indicated that the model was significant. The “Lack of Fit F -value” is used to represent the degree of fitting between the model and the experiment, and the “Lack of Fit F -value” of 6.14 (>0.05) implied it was insignificant, which implied that the RSM model fitted the experimental data well [26,27]. For the model fitting, the coefficient of determination ( R 2 ) was 0.9389, indicating that only 6.11% of the total variation was not suitable according to the model.…”

Structural Determination and Genetic Identification of the O-Antigen from an Escherichia coli Strain, LL004, Representing a Novel Serogroup

“…The extra acid was completely removed by adding methanol with rotary evaporation [ 25 ]. The monosaccharides were analysed by high-performance anion-exchange chromatography coupled with pulsed amperometric detection (HPAEC–PAD) method [ 26 ]. HPAEC–PAD analysis was performed using an ICS-5000+ ion chromatography system that consisted of a quaternary pump, temperature-controlled column manager, and ED5000 PAD electrochemical cell which consisted of an Au working electrode and pH-Ag/AgCl reference electrode.…”

Recent liquid chromatographic approaches and developments for the separation and purification of carbohydrates

“…This interface resulted in greater ionization efficiency of mono/di-saccharides for the analysis of neutral sugars in pectin samples that were separated with HPAEC 66 . In another study, 13 monosaccharides from polysaccharide from Arthrospira ( Spirulina) platensis (both neutral ones and acidic, carboxy, sugars that are already negatively charged at neutral pH) were simultaneously separated through a gradient elution of sodium hydroxide and sodium acetate with HPAEC coupled to both PAD and MS detectors 67 . Although separation of the neutral monosaccharides can be increased when a lower pH is used for the alkaline eluent since both neutral and acidic, carboxylated, sugars were analyzed, it was found that a higher concentration of NaOH was necessary for the desired separation 67 .…”