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Development, Validation, Innovative Analytical Approaches in the Study of Food...
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Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (31 July 2022) | Viewed by 16210

Special Issue Editors

Dr. Stefano Dall'Acqua

E-Mail Website
Guest Editor
Pharmaceutical and Pharmacological Sciences, Universita degli Studi di Padova, Padua, Italy
Interests: bioactive natural products; terpenoids; phenolics; saponins; alkaloids; NMR; LC-MS; GC-MS
Special Issues, Collections and Topics in MDPI journals
Dr. Stefania Sut

E-Mail Website1 Website2
Guest Editor
Department of medicine, University of Padova, 35121 Padova, Italy
Interests: bioactive natural compounds; natural product chemistry; analysis of natural product; mass spectrometry; NMR; secondary metabolites in plant; analytical techniques; complex mixtures

Special Issue Information

Dear Colleagues,

The large diffusion of food supplements and nutraceuticals opens new questions related to products’ quality and composition. Analytical approaches to assess quality and stability of such compounds are required and can be useful during product development, quality control, and to assess their safety.

This Special Issue will collect contributions in the analytical determination of nutraceutical and food supplements.

Paper dealing with analytical approaches for the determination of bioactive constituents as botanicals, plant oils, fish oils, aminoacids, proteins, fibers, and polymers and all kinds of active constituents will be welcomed. All papers dealing with well-known ingredients such as vitamins or other nutritional factors will be considered if presenting innovation in analytical procedures and special application to specific products or matrices (syrups, juices, tablets, etc.). Methods for the analysis of final products with attention to stability studies, studies related to formulations, and interactions of active constituents with excipients will be welcomed. Studies related to the development of methods for the analysis of undesired compounds will be considered if novel in approach or in findings.

This Special Issue aims to collect the most feasible and useful analytical approaches for accurate quantification of bioactive compounds in food supplements and nutraceuticals.

Dr. Stefano Dall'Acqua
Dr. Stefania Sut
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • botanicals
  • vitamins
  • spectrophotometry
  • FT-IR
  • NIR
  • Raman spectroscopy
  • NMR spectroscopy
  • mass spectrometry
  • chromatography
  • HPLC
  • UPLC
  • GC
  • LC
  • GC-MS
  • LC-MS
  • LC-NMR

Published Papers (6 papers)

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Research

19 pages, 2289 KiB  
Article
Development, Validation, and Use of 1H-NMR Spectroscopy for Evaluating the Quality of Acerola-Based Food Supplements and Quantifying Ascorbic Acid
by Asma Bourafai-Aziez, Daniel Jacob, Gwladys Charpentier, Emmanuel Cassin, Guillaume Rousselot, Annick Moing and Catherine Deborde
Molecules 2022, 27(17), 5614; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27175614 - 31 Aug 2022
Cited by 3 | Viewed by 3993
Abstract
Acerola (Malpighia emarginata D.C.) is an exotic fruit with high agro-industrial potential due to its high content of ascorbic acid (AA), phenolic compounds, and carotenoid pigments. Acerola fruit is processed into concentrated juice or powder to be incorporated into food supplements. The [...] Read more.
Acerola (Malpighia emarginata D.C.) is an exotic fruit with high agro-industrial potential due to its high content of ascorbic acid (AA), phenolic compounds, and carotenoid pigments. Acerola fruit is processed into concentrated juice or powder to be incorporated into food supplements. The ascorbic acid content of concentrated juice or powders must be controlled and well assessed. Therefore, the development of optimal methods and procedures for the rapid and accurate determination of the ascorbic acid content in juice concentrate and juice powder remains of considerable commercial interest. NMR spectroscopy is currently a powerful spectroscopic tool for the qualitative and quantitative analysis of molecules of all types and sizes. Firstly, this article presents the NMR-based metabolomic profiling of acerola juice and concentrate powder to describe and compare their composition. Thirty-six metabolites were identified. The AA over choline ratio and the NMR metabolomic profiles could be used for authentication in the future. Secondly, a rapid (8 min), reliable, and non-destructive method for the quantification of ascorbic acid by 1D 1H-NMR spectroscopy was developed and validated. The LOD and LOQ were 0.05 and 0.15 mg/mL, respectively. These two approaches could be combined to better characterize ingredients derived from acerola and incorporated into food supplements. Full article
(This article belongs to the Special Issue Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition)
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14 pages, 901 KiB  
Article
Development and Validation of the UPLC-DAD Methodology for the Detection of Triterpenoids and Phytosterols in Fruit Samples of Vaccinium macrocarpon Aiton and Vaccinium oxycoccos L.
by Rima Sedbare, Lina Raudone, Vaidotas Zvikas, Jonas Viskelis, Mindaugas Liaudanskas and Valdimaras Janulis
Molecules 2022, 27(14), 4403; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27144403 - 09 Jul 2022
Cited by 11 | Viewed by 1563
Abstract
Cranberries are used in the production of medicinal preparations and food supplements, which highlights the importance of triterpene compounds determination in cranberry fruit raw material. The aim of our study was to develop and validate for routine testing suitable UPLC-DAD methodology for the [...] Read more.
Cranberries are used in the production of medicinal preparations and food supplements, which highlights the importance of triterpene compounds determination in cranberry fruit raw material. The aim of our study was to develop and validate for routine testing suitable UPLC-DAD methodology for the evaluation of triterpene acids, neutral triterpenoids, phytosterols, and squalene content in cranberry samples. The developed and optimized UPLC-DAD methodology was validated according to the guidelines of the International Council for Harmonization (ICH), evaluating the following parameters: range, specificity, linearity (R2 > 0.999), precision, LOD (0.27–1.86 µg/mL), LOQ (0.90–6.18 µg/mL), and recovery (80–110%). The developed and validated technique was used for the evaluation of triterpenic compounds in samples of Vaccinium macrocarpon and Vaccinium oxycoccos fruits, and their peels, pulp and seeds. The studied chromatogram profiles of Vaccinium macrocarpon and Vaccinium oxycoccos were identical but differed in the areas of the analytical peaks. Ursolic acid was the dominant compound in fruit samples of Vaccinium macrocarpon and Vaccinium oxycoccos. The highest amounts of triterpenic compounds were detected in the cranberry peels samples. The developed method for the detection of triterpene compounds can be applied in further studies for routine testing on the qualitative and quantitative composition of fruit samples of Vaccinium macrocarpon and Vaccinium oxycoccos species and cultivars. Full article
(This article belongs to the Special Issue Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition)
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12 pages, 2394 KiB  
Article
Development of an LC–DAD–MS-Based Method for the Analysis of Hydroxyanthracene Derivatives in Food Supplements and Plant Materials
by Francesca Loschi, Marta Faggian, Stefania Sut, Irene Ferrarese, Erica Maccari, Gregorio Peron and Stefano Dall’Acqua
Molecules 2022, 27(6), 1932; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27061932 - 16 Mar 2022
Cited by 3 | Viewed by 2328
Abstract
Products based on plants containing hydroxyanthracene derivatives (HADs)—such as Rheum, Cassia, and Aloe species—are widely used in food supplements or nutraceuticals due to their laxative effects. A more restricted control of HAD contents in food supplements has been implemented by EU [...] Read more.
Products based on plants containing hydroxyanthracene derivatives (HADs)—such as Rheum, Cassia, and Aloe species—are widely used in food supplements or nutraceuticals due to their laxative effects. A more restricted control of HAD contents in food supplements has been implemented by EU Regulation 2021/468, in order to increase the safety of these preparations. Due to their toxicity, aloin A, aloin B, aloe emodin, emodin, and the synthetic derivative danthron have been listed as prohibited substances in food supplements, being tolerated in amounts < 1 mg kg−1 in marketed products. In this work, we report the development of a sensitive and fast LC–DAD–MS-based procedure for the determination of these five compounds in food supplements and plant materials or extracts. The entire procedure includes a simple sample preparation step, where target analytes are concentrated by means of solvent extraction and evaporative concentration (solid samples), or by lyophilisation (liquid samples). The average LOQ of 0.10 mg/L, LOD of 0.03 mg/L, accuracy, and precision with CVs below 12.72 were obtained for the studied analytes. This method is suitable for assessing the compliance of commercial products and raw materials with EU Regulation 2021/468. Furthermore, the proposed method can represent a starting point for the development of a unique and standardised analytical approach for the determination of other HADs under the attention of EU authorities. Full article
(This article belongs to the Special Issue Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition)
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16 pages, 855 KiB  
Article
Development, Validation, and Application of the UPLC-DAD Methodology for the Evaluation of the Qualitative and Quantitative Composition of Phenolic Compounds in the Fruit of American Cranberry (Vaccinium macrocarpon Aiton)
by Rima Urbstaite, Lina Raudone, Mindaugas Liaudanskas and Valdimaras Janulis
Molecules 2022, 27(2), 467; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules27020467 - 12 Jan 2022
Cited by 8 | Viewed by 1966
Abstract
Phenolic compounds in the fruit of American cranberry (Vaccinium macrocarpon Aiton) determine the antioxidant, anti-inflammatory, anticancer, and other biological effects. The berries are used in the production of medicinal preparations and food supplements, which highlights the importance of qualitative and quantitative analysis [...] Read more.
Phenolic compounds in the fruit of American cranberry (Vaccinium macrocarpon Aiton) determine the antioxidant, anti-inflammatory, anticancer, and other biological effects. The berries are used in the production of medicinal preparations and food supplements, which highlights the importance of qualitative and quantitative analysis of phenolic compounds in cranberry fruit raw material. The aim of our study was to develop and validate an efficient, cost-effective, reproducible, and fast UPLC-DAD methodology for the evaluation of the qualitative and quantitative composition of phenolic compounds in raw material and preparations of American cranberry fruit. During the development of the methodology, chlorogenic acid and the following flavonols were identified in cranberry fruit samples: myricetin-3-galactoside, quercetin-3-galactoside, quercetin-3-glucoside, quercetin-3-α-L-arabinopyranoside, quercetin-3-α-L-arabinofuranoside, quercetin-3-rhamnoside, myricetin, and quercetin. The developed and optimized UPLC-DAD methodology was validated according to the guidelines of the International Council for Harmonization (ICH), evaluating the following parameters: range, specificity, linearity (R2 > 0.999), precision (%RSD < 2%), LOD (0.38–1.01 µg/mL), LOQ (0.54–3.06 µg/mL), and recovery (80–110%). The developed methodology was applied to evaluate the qualitative and quantitative composition of phenolic compounds in fruit samples of cranberry cultivars ‘Baifay’, ‘Bergman’, ‘Prolific’, and ‘Searles’, as well as ‘Bain-MC’ and ‘BL-12′ clones. In the tested samples, the majority (about 70%) of the identified flavonols were quercetin derivatives. The greatest amount of quercetin-3-galactoside (1035.35 ± 4.26 µg/g DW) was found in fruit samples of the ‘Searles’ cultivar, and the greatest amount of myricetin-3-galactoside (940.06 ± 24.91 µg/g DW) was detected in fruit samples of the ‘Woolman’ cultivar. Full article
(This article belongs to the Special Issue Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition)
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12 pages, 1449 KiB  
Article
Simultaneous Determination of Vitamins D3 (Calcitriol, Cholecalciferol) and K2 (Menaquinone-4 and Menaquinone-7) in Dietary Supplements by UHPLC
by Anca Becze, Vanda Liliana Babalau Fuss, Daniela Alexandra Scurtu, Maria Tomoaia-Cotisel, Aurora Mocanu and Oana Cadar
Molecules 2021, 26(22), 6982; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26226982 - 19 Nov 2021
Cited by 3 | Viewed by 2474
Abstract
The content and composition of dietary supplements is of great interest due to their increasing consumption and variety of available brand offered in the market. Accurate determination of vitamins is important for the improvement of dietary supplement quality and nutrition assessments. In this [...] Read more.
The content and composition of dietary supplements is of great interest due to their increasing consumption and variety of available brand offered in the market. Accurate determination of vitamins is important for the improvement of dietary supplement quality and nutrition assessments. In this regard, the simultaneous determination of vitamin D3 (calcitriol—CT and cholecalciferol—CHL) and K2 (menaquinone-4—MK-4 and menaquinone-7—MK-7) in dietary supplements was developed by using ultra-high-pressure liquid chromatography (UHPLC). The overall runtime per sample was above 35 min, with the retention times of 2.40, 6.59, 7.06, and 32.6 min for vitamin D3 (CT and CHL) and vitamin K2 (MK-4 and MK-7), respectively. The limits of detection and limits of quantification for the target nutritional compounds ranged between 0.04–0.05 µg/mL, respectively. The validation results indicated that the method had reasonable linearity (R2 ≥ 0.9990), good recovery (>82%), satisfactory intra-day precision (≤1.9%) and inter-day precision (≤3.5%), and high selectivity and specificity. The validated UHPLC method was demonstrated to be precise, accurate, and robust for the simultaneous determination of vitamins D3 (CT and CHL) and K2 (MK-4 and MK-7) in dietary supplements. Full article
(This article belongs to the Special Issue Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition)
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11 pages, 791 KiB  
Article
Analysis of Monacolins and Berberine in Food Supplements for Lipid Control: An Overview of Products Sold on the Italian Market
by Sara Marcheluzzo, Marta Faggian, Mirella Zancato and Gregorio Peron
Molecules 2021, 26(8), 2222; https://0-doi-org.brum.beds.ac.uk/10.3390/molecules26082222 - 12 Apr 2021
Cited by 6 | Viewed by 2724
Abstract
The use of dietary supplements for the prevention and management of diseases associated with excess of lipids is spreading in Western countries. Supplements containing red yeast rice (RYR) and extracts from Berberis species, characterized, respectively, by the active compounds monacolin K (MK) and [...] Read more.
The use of dietary supplements for the prevention and management of diseases associated with excess of lipids is spreading in Western countries. Supplements containing red yeast rice (RYR) and extracts from Berberis species, characterized, respectively, by the active compounds monacolin K (MK) and berberine (BBR), are sold in pharmacies as over the counter medicines (OTC) and in regular markets without the need of medical prescription and medical surveillance. However, MK is chemically identical to lovastatin, a drug commonly used to treat hypercholesterolemia, and is characterized by the same mechanism of action, pharmacokinetic profile and toxicity. On the other hand, although BBR-containing supplements are considered to be well-tolerated and safe, they frequently show poor standardization of active ingredients, and this could lead to lack of effects. In this work, with the aim to give an overview on the potency of RYR- and BBR-containing supplements available on the Italian market, we analyzed a pool of supplements bought from both local pharmacies and markets. Results confirm the data already published by other authors, showing scarce standardization of bioactives and discrepancy between the doses of bioactives reported by the manufacturers and the amounts resulting from analysis of the same products. Overall, our data represent a further proof that a strict legislation regulating the production and marketing of dietary supplements and a close monitoring of these products by food and drug regulatory organs is mandatory. Full article
(This article belongs to the Special Issue Development, Validation, Innovative Analytical Approaches in the Study of Food Supplement and Nutraceutical Composition)
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