Quantification of food polysaccharide mixtures by 1H NMR

Merkx, Donny W.H.; Westphal, Yvonne; Velzen, Ewoud J. J. van; Thakoer, Kavish V.; Roo, Niels de; Duynhoven, John van

doi:10.1016/j.carbpol.2017.09.074

Cited by 42 publications

(22 citation statements)

References 19 publications

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“…Quantitative NMR has become a widely used analytical tool for the quantification of polysaccharides, being an important tool when evaluating the chemistry of these polymers [20]. In our study, the chemical modification of Kefiran was assessed by 1 H-NMR (Figure 1a).…”

Section: H-nmrmentioning

confidence: 99%

Synthesis and Characterization of Biocompatible Methacrylated Kefiran Hydrogels: Towards Tissue Engineering Applications

et al. 2021

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Hydrogel application feasibility is still limited mainly due to their low mechanical strength and fragile nature. Therefore, several physical and chemical cross-linking modifications are being used to improve their properties. In this research, methacrylated Kefiran was synthesized by reacting Kefiran with methacrylic anhydride (MA). The developed MA-Kefiran was physicochemically characterized, and its biological properties evaluated by different techniques. Chemical modification of MA-Kefiran was confirmed by 1H-NMR and FTIR and GPC-SEC showed an average Mw of 793 kDa (PDI 1.3). The mechanical data obtained revealed MA-Kefiran to be a pseudoplastic fluid with an extrusion force of 11.21 ± 2.87 N. Moreover, MA-Kefiran 3D cryogels were successfully developed and fully characterized. Through micro-CT and SEM, the scaffolds revealed high porosity (85.53 ± 0.15%) and pore size (33.67 ± 3.13 μm), thick pore walls (11.92 ± 0.44 μm) and a homogeneous structure. Finally, MA-Kefiran revealed to be biocompatible by presenting no hemolytic activity and an improved cellular function of L929 cells observed through the AlamarBlue® assay. By incorporating methacrylate groups in the Kefiran polysaccharide chain, a MA-Kefiran product was developed with remarkable physical, mechanical, and biological properties, resulting in a promising hydrogel to be used in tissue engineering and regenerative medicine applications.

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Section: H-nmrmentioning

confidence: 99%

Synthesis and Characterization of Biocompatible Methacrylated Kefiran Hydrogels: Towards Tissue Engineering Applications

et al. 2021

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“…There were also less performing chromatographic techniques with higher limits of quantification, such as GC-FID (2) and TLC, where the limits of quantification were on the order of one thousand of log. It would have been interesting to study the limits of quantification at the polymer scale (g monosaccharide/100 g polysaccharides) as developed for NMR methods for polysaccharides [24] and food matrices [25].…”

Section: Analytical Performance Of the Methodsmentioning

confidence: 99%

“…Different methods based on the use of nuclear magnetic resonance (NMR) systems have been developed to quantify or to profile polysaccharides. Studies have shown that the use of 1 H NMR, when preceded by the Saeman hydrolysis procedure [23], could identify and quantify the osidic monomer composition of the main food polysaccharides (high acyl gellan, xanthan, pectins, and locust bean gum) [24]. With other NMR approaches based on the chemical-shift-selective filtration with total correlation spectroscopy (CSSF-TOCSY) sequence, 22 different saccharides can be distinguished simultaneously in an aqueous medium without pre-treatment, even if they are in the form of a monomer (glucose), dimer (sucrose), or trimer (raffinose).…”

Section: Introductionmentioning

confidence: 99%

A New, Quick, and Simple Protocol to Evaluate Microalgae Polysaccharide Composition

et al. 2021

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In this work, a new methodological approach, relying on the high specificity of enzymes in a complex mixture, was developed to estimate the composition of bioactive polysaccharides produced by microalgae, directly in algal cultures. The objective was to set up a protocol to target oligomers commonly known to be associated with exopolysaccharides’ (EPS) nutraceutical and pharmaceutical activities (i.e., rhamnose, fucose, acidic sugars, etc.) without the constraints classically associated with chromatographic methods, while maintaining a resolution sufficiently high to enable their monitoring in the culture system. Determination of the monosaccharide content required the application of acid hydrolysis (2 M trifluoroacetic acid) followed by NaOH (2 M) neutralization. Quantification was then carried out directly on the fresh hydrolysate using enzyme kits corresponding to the main monosaccharides in a pre-determined composition of the polysaccharides under analysis. Initial results showed that the enzymes were not sensitive to the presence of TFA and NaOH, so the methodology could be carried out on fresh hydrolysate. The limits of quantification of the method were estimated as being in the order of the log of nanograms of monosaccharides per well, thus positioning it among the chromatographic methods in terms of analytical performance. A comparative analysis of the results obtained by the enzymatic method with a reference method (high-performance anion-exchange chromatography) confirmed good recovery rates, thus validating the closeness of the protocol. Finally, analyses of raw culture media were carried out and compared to the results obtained in miliQ water; no differences were observed. The new approach is a quick, functional analysis method allowing routine monitoring of the quality of bioactive polysaccharides in algal cultures grown in photobioreactors.

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“…For the aqueous fraction, and according to its proton spectrum (Fig. 3S), it presents signals corresponding to polyphenolic compounds (7.5-6.5 ppm) (Apaza Ticona et al 2021), polysaccharides (5.5-3.5 ppm) (Merkx et al 2018), fatty acids (2.5-1.0 ppm) (Castejón et al 2016), being the polysaccharides are in higher proportion. In the case of n-C 7 H 16 fraction, the presence of fatty acids (2.5-1 ppm) in the proton spectrum (Fig.…”

Section: Inhibition Of Tnf-α Productionmentioning

confidence: 99%

Anti-inflammatory and Anti-arthritic Activities of Glycosylated Flavonoids from Syzygium jambos in Edematogenic Agent-Induced Paw Edema in Mice

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et al. 2021

Rev. Bras. Farmacogn.

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Two glycosylated flavonoids, the quercetin-3-O-β-d-xylofuranosyl-(1 → 2)-α-l-rhamnopyranoside and myricetin-3-O-β-d-xylofuranosyl-(1 → 2)-α-l-rhamnopyranoside, were isolated from the CH2Cl2/MeOH fraction of Syzygium jambos (L.) Alston, Myrtaceae. The structures of these compounds were elucidated by spectroscopic means. The cytotoxicity of the compounds was evaluated against the RAW 264.7 cell lines by the lactate dehydrogenase assay. All analyzed compounds were less cytotoxic than the positive control (actinomycin D, CC50 = 0.008 μM). The anti-inflammatory and anti-arthritic activities were evaluated by measuring inflammatory parameters in murine models. The two glycosylated flavonoids inhibited the production of tumor necrosis factor-α in RAW 264.7 cell line with IC50 of 1.68 and 1.11 μM, respectively. In addition, all flavonoids decreased the levels of tumor necrosis factor-α, C-reactive protein, and fibrinogen at a dose of 5 mg/kg in murine models. Graphical abstract

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Quantification of food polysaccharide mixtures by 1H NMR

Cited by 42 publications

References 19 publications

Synthesis and Characterization of Biocompatible Methacrylated Kefiran Hydrogels: Towards Tissue Engineering Applications

Synthesis and Characterization of Biocompatible Methacrylated Kefiran Hydrogels: Towards Tissue Engineering Applications

A New, Quick, and Simple Protocol to Evaluate Microalgae Polysaccharide Composition

Anti-inflammatory and Anti-arthritic Activities of Glycosylated Flavonoids from Syzygium jambos in Edematogenic Agent-Induced Paw Edema in Mice

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