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Special Issue "Advances in Liquid Separation Techniques for Food and Pharmaceutical Analysis"

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

Deadline for manuscript submissions: 31 August 2018

Special Issue Editors

Guest Editor
Dr. Nicola Marchetti

Department of Chemistry and Pharmaceutical Sciences, University of Ferrara, via Fossato di Mortara, 17/19, I-44121 Ferrara, Italy
Website | E-Mail
Interests: HPLC, LC–MS, natural bioactive compounds, food chemistry, nutraceutics, gastrointestinal bioaccessibility
Guest Editor
Dr. Anna Laura Capriotti

Department of Chemistry, University of Rome, La Sapienza, Piazzale Aldo Moro, 5, 00185, Roma, Italy
Website | E-Mail
Interests: HPLC, LC–MS, sample preparation, bioactive peptides, natural bioactive compounds, proteomics and peptidomics

Special Issue Information

Dear Colleagues,

Today, the demand for highly efficient, selective, sensitive, reproducible and green analytical methodologies for complex sample preparation, fractionation and/or extraction of bioactive compounds, analysis and chemical characterization, requires continuous advances in separation media, adsorbent materials and detection techniques. All these aspects belong to analytical methodologies where liquid separation techniques play the major role.

The main aims of the present Special Issue on "Advances in Liquid Separation Techniques for Food and Pharmaceutical Analysis" belong to both fundamental studies and real case multidisciplinary investigations. Contributions to this issue, both in the form of original research or review articles, have the broad scope to illustrate recent and future trends of liquid chromatography and hyphenated techniques offering a clear vision and insights for new methodologies, improving instrumental performances and providing sensitivity and specificity.

Innovative approaches in the field of pharmaceutical sciences, cosmetics, nutraceutics, food chemistry, finalized to the extraction, characterization, purification and validation of chiral or achiral active pharmaceutical ingredients, and natural bioactive compounds from plants, are particularly welcome. Also of interest would be studies concerning molecules that are obtained from waste and re-used as secondary raw materials. Studies that involve UPLC, SFC and their hyphenation with mass spectrometry are also strongly encouraged.

Dr. Nicola Marchetti
Dr. Anna Laura Capriotti
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 papers will be 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 monthly 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 1800 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

  • HPLC-, UPLC-, SFC-MS
  • Sample preparation
  • Food bioactive compounds
  • Active pharmaceutical ingredients
  • Purification/extraction techniques
  • Bioanalytics
  • Nutraceutics

Published Papers (13 papers)

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Research

Open AccessArticle Development of Validated and Stability-Indicating LC-DAD and LC-MS/MS Methods for Determination of Avanafil in Pharmaceutical Preparations and Identification of a Novel Degradation Product by LCMS-IT-TOF
Molecules 2018, 23(7), 1771; https://doi.org/10.3390/molecules23071771
Received: 11 June 2018 / Revised: 9 July 2018 / Accepted: 13 July 2018 / Published: 19 July 2018
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Abstract
Avanafil (AVA), one of the most effective drugs prescribed for erectile dysfunction, is a pyrimidine-derivative PDE5 inhibitor. In the current work, new LC methods were developed and validated for quantitative determination of avanafil and qualitative determination of its degradation products. The quantitative determination
[...] Read more.
Avanafil (AVA), one of the most effective drugs prescribed for erectile dysfunction, is a pyrimidine-derivative PDE5 inhibitor. In the current work, new LC methods were developed and validated for quantitative determination of avanafil and qualitative determination of its degradation products. The quantitative determination of avanafil was carried out using liquid chromatography with photodiode array detection (LC-DAD) and liquid chromatography-tandem mass spectrometry LC-MS/MS methods, and fully validated according to the ICH Q2 (R1) guideline, while qualitative determination was performed using a liquid chromatography mass spectrometry-ion trap-time of flight (LCMS-IT-TOF) instrument. The separation of avanafil and its degradation products was carried out using the same reversed-phase chromatographic conditions, in which a second-generation C18-bonded monolithic silica column (Chromolith® High Resolution RP-18e, 100 × 4.6 mm, Merck KGaA) was used as stationary phase. Briefly, the methods enable quantitation of avanafil with high accuracy (recovery > 95%) and precision (RSD% < 2.0), within the ranges of 0.5–20 μg/mL for LC-DAD and 150–6000 ng/mL for LC-MS/MS. In the forced degradation studies, over and above currently existing data, a new oxidation-based degradation product, whose predicted m/z is 367.1168, was identified and its structure was confirmed by high-resolution mass spectrometric analysis. As the main advantage, either an LC-DAD or LC-MS/MS instrument can be chosen for interference-free quantitation of AVA, according to the facilities in quality-control laboratories. Full article
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Open AccessArticle Aflatoxins and A. flavus Reduction in Loaf Bread through the Use of Natural Ingredients
Molecules 2018, 23(7), 1638; https://doi.org/10.3390/molecules23071638
Received: 6 June 2018 / Revised: 28 June 2018 / Accepted: 3 July 2018 / Published: 4 July 2018
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Abstract
In this study, the antifungal activity of yellow mustard (YMF) and oriental mustard (OMF) meal extracts against 14 strains of fungi was tested on a solid medium. The results obtained with the YMF were next confirmed in liquid medium determining the minimum inhibitory
[...] Read more.
In this study, the antifungal activity of yellow mustard (YMF) and oriental mustard (OMF) meal extracts against 14 strains of fungi was tested on a solid medium. The results obtained with the YMF were next confirmed in liquid medium determining the minimum inhibitory concentration (MIC) and the minimum fungicide concentration (MFC). Finally, the use of YMF as a natural preservative to extend the useful life of bread was evaluated. Breads with different concentrations of YMF (2, 4, 6 and 8 g/kg) were prepared and contaminated with Aspergillus flavus ISPA 8111 and Penicillium nordicum CECT 2320. For 10 days the formation of mycelium was observed, and after that the fungal growth and the mycotoxins production was determined. The results obtained with the YMF were compared with breads treated with the commercial additive sodium propionate (E-281). The results showed a significant reduction of the fungal population using 6 g/kg and 8 g/kg of YMF in bread contaminated with A. flavus and with P. nordicum and an extensions of the breads shelf life of 7 and 5 days, respectively, in comparison with the control experiment. A reduction of 78% of AFB1 was observed using 6 g/kg of YMF while no AFB1 production was detected employing 8 g/kg of YMF in bread preparation. Full article
Open AccessArticle Upregulation of UDP-Glucuronosyltransferases 1a1 and 1a7 Are Involved in Altered Puerarin Pharmacokinetics in Type II Diabetic Rats
Molecules 2018, 23(6), 1487; https://doi.org/10.3390/molecules23061487
Received: 1 June 2018 / Revised: 17 June 2018 / Accepted: 17 June 2018 / Published: 20 June 2018
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Abstract
Puerarin is an isoflavonoid extracted from Pueraria lobata roots, and displays a broad range of pharmacological activities, including antidiabetic activity. However, information about the pharmacokinetics of puerarin in diabetics is scarce. This study was conducted to investigate the difference in pharmacokinetic effects of
[...] Read more.
Puerarin is an isoflavonoid extracted from Pueraria lobata roots, and displays a broad range of pharmacological activities, including antidiabetic activity. However, information about the pharmacokinetics of puerarin in diabetics is scarce. This study was conducted to investigate the difference in pharmacokinetic effects of puerarin in normal rats and rats with diabetes mellitus (DM), and the mechanism involved. DM was induced by a combined high-fat diet (HFD) and streptozotocin (STZ) injection. Plasma concentrations of puerarin in DM, HFD, and control rats were determined after intravenous (20 mg/kg) and oral administration (500 mg/kg) of puerarin, and pharmacokinetic parameters were estimated. The messenger RNA (mRNA) and protein expression levels of Ugt1a1 and Ugt1a7 in rat livers and intestines were measured using qRT-PCR and western blot, respectively. The area under the concentration–time curve and the clearance of puerarin in the DM rats statistically differed from those in the control rats (p <0.05) with both administration routes. The hepatic and intestinal gene and protein expressions of Ugt1a1 and Ugt1a7 were significantly increased in the DM rats (p <0.05). Therefore, the metabolic changes in diabetes could alter the pharmacokinetics of puerarin. This change could be caused by upregulated uridine diphosphate (UDP)-glucuronosyltransferase activity, which may enhance puerarin clearance, and alter its therapeutic effects. Full article
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Open AccessArticle Plasma Pharmacokinetic Determination of Canagliflozin and Its Metabolites in a Type 2 Diabetic Rat Model by UPLC-MS/MS
Molecules 2018, 23(5), 1229; https://doi.org/10.3390/molecules23051229
Received: 3 May 2018 / Revised: 15 May 2018 / Accepted: 17 May 2018 / Published: 20 May 2018
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Abstract
Canagliflozin is a novel, orally selective inhibitor of sodium-dependent glucose co-transporter-2 (SGLT2) for the treatment of patients with type 2 diabetes mellitus. In this study, a sensitive and efficient UPLC-MS/MS method for the quantification of canagliflozin and its metabolites in rat plasma was
[...] Read more.
Canagliflozin is a novel, orally selective inhibitor of sodium-dependent glucose co-transporter-2 (SGLT2) for the treatment of patients with type 2 diabetes mellitus. In this study, a sensitive and efficient UPLC-MS/MS method for the quantification of canagliflozin and its metabolites in rat plasma was established and applied to pharmacokinetics in a type 2 diabetic rat model. We firstly investigated the pharmacokinetic changes of canagliflozin and its metabolites in type 2 diabetic rats in order to use canagliflozin more safely, reasonably and effectively. We identified three types of O-glucuronide metabolites (M5, M7 and M17), two kinds of oxidation metabolites (M8 and M9) and one oxidation and glucuronide metabolite (M16) using API 5600 triple-TOF-MS/MS. Following liquid–liquid extraction by tert-butyl methyl ether, chromatographic separation of canagliflozin and its metabolites were performed on a Waters XBridge BEH C18 column (100 × 2.1 mm, 2.5 μm) using 0.1% acetonitrile–formic acid (75:15, v/v) as the mobile phase at a flow rate of 0.7 mL/min. Selected ion monitoring transitions of m/z 462.00→191.10, 451.20→153.10, 638.10→191.10 and 478.00→267.00 were chosen to quantify canagliflozin, empagliflozin (IS), O-glucuronide metabolites (M5, M7 and M17), and oxidation metabolites (M9) using an API 5500-triple-MS/MS in the positive electrospray ionization mode. The validation of the method was found to be of sufficient specificity, accuracy and precision. The pathological condition of diabetes could result in altered pharmacokinetic behaviors of canagliflozin and its metabolites. The pharmacokinetic parameters (AUC0–t, AUC0–∞, CLz/F, and Vz/F) of canagliflozin were significantly different between the CTRL and DM group rats (p < 0.05 or p < 0.01), which may subsequently cause different therapeutic effects. Full article
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Open AccessArticle Antioxidant and ACE Inhibitory Activity of Enzymatic Hydrolysates from Ruditapes philippinarum
Molecules 2018, 23(5), 1189; https://doi.org/10.3390/molecules23051189
Received: 13 April 2018 / Revised: 3 May 2018 / Accepted: 8 May 2018 / Published: 16 May 2018
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Abstract
Ruditapes philippinarum proteins were hydrolyzed by trypsin, neutrase, and pepsin. The antioxidant activities and ACE inhibitory activity of hydrolysates were analyzed and the antioxidant activities were related to their molecular weight distribution and amino acid compositions. Results indicated the hydrolysis of proteins led
[...] Read more.
Ruditapes philippinarum proteins were hydrolyzed by trypsin, neutrase, and pepsin. The antioxidant activities and ACE inhibitory activity of hydrolysates were analyzed and the antioxidant activities were related to their molecular weight distribution and amino acid compositions. Results indicated the hydrolysis of proteins led to an increase in small peptides and free amino acids. The antioxidant activities of Ruditapes philippinarum hydrolysates against DPPH radical scavenging, inhibition on linoleic acid peroxidation, and reducing power showed that the neutrase hydrolysate exhibited the strongest antioxidant activity. In addition, an ACE inhibition assay revealed that the pepsin hydrolysate had the highest ACE inhibitory ability. Ruditapes philippinarum protein hydrolysates could be a promising source of natural antioxidant and ACE inhibitory. Full article
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Open AccessFeature PaperArticle Fast Profiling of Natural Pigments in Different Spirulina (Arthrospira platensis) Dietary Supplements by DI-FT-ICR and Evaluation of their Antioxidant Potential by Pre-Column DPPH-UHPLC Assay
Molecules 2018, 23(5), 1152; https://doi.org/10.3390/molecules23051152
Received: 20 April 2018 / Revised: 2 May 2018 / Accepted: 10 May 2018 / Published: 11 May 2018
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Abstract
Arthrospira platensis, better known as Spirulina, is one of the most important microalgae species. This cyanobacterium possesses a rich metabolite pattern, including high amounts of natural pigments. In this study, we applied a combined strategy based on Fourier Transform Ion Cyclotron Resonance
[...] Read more.
Arthrospira platensis, better known as Spirulina, is one of the most important microalgae species. This cyanobacterium possesses a rich metabolite pattern, including high amounts of natural pigments. In this study, we applied a combined strategy based on Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR-MS) and Ultra High-Performance Liquid Chromatography (UHPLC) for the qualitative/quantitative characterization of Spirulina pigments in three different commercial dietary supplements. FT-ICR was employed to elucidate the qualitative profile of Spirulina pigments, in both direct infusion mode (DIMS) and coupled to UHPLC. DIMS showed to be a very fast (4 min) and accurate (mass accuracy ≤ 0.01 ppm) tool. 51 pigments were tentatively identified. The profile revealed different classes, such as carotenes, xanthophylls and chlorophylls. Moreover, the antioxidant evaluation of the major compounds was assessed by pre-column reaction with the DPPH radical followed by fast UHPLC-PDA separation, highlighting the contribution of single analytes to the antioxidant potential of the entire pigment fraction. β-carotene, diadinoxanthin and diatoxanthin showed the highest scavenging activity. The method took 40 min per sample, comprising reaction. This strategy could represent a valid tool for the fast and comprehensive characterization of Spirulina pigments in dietary supplements, as well as in other microalgae-based products. Full article
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Open AccessArticle Quantitative Analysis of Four Catechins from Green Tea Extract in Human Plasma Using Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry for Pharmacokinetic Studies
Molecules 2018, 23(4), 984; https://doi.org/10.3390/molecules23040984
Received: 28 February 2018 / Revised: 15 April 2018 / Accepted: 19 April 2018 / Published: 23 April 2018
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Abstract
Green tea is consumed as a beverage worldwide and has beneficial effects, such as a lower risk of cardiovascular disease and cancer. A quantitative analysis of the beneficial components in plasma is important for understanding the potential health benefits of green tea. Four
[...] Read more.
Green tea is consumed as a beverage worldwide and has beneficial effects, such as a lower risk of cardiovascular disease and cancer. A quantitative analysis of the beneficial components in plasma is important for understanding the potential health benefits of green tea. Four catechins—epigallocatechin-3-gallate (EGCG), epicatechin-3-gallate (ECG), epigallocatechin (EGC), and epicatechin (EC)—which account for the majority of the components of green tea, were analyzed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). In this study, a validated method was optimized to obtain the blood concentrations after the one-time ingestion of 630 mg green tea extract with digoxin and then after the ingestion of 630 mg green tea repeatedly for 15 days. The calibration curve, including the LLOQ, was constructed over 1–500 ng/mL for EGCG, ECG, and EGC and 0.1–50 ng/mL for EC. The method for inter- and intra-validation was applied, acceptable for both accuracy and precision. We successfully developed an appropriate UPLC-MS/MS method for human plasma with good reproducibility and sensitivity. Thus, this method could be applied for future preclinical and clinical studies on EGCG, ECG, EGC, and EC. Full article
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Open AccessArticle Single Laboratory Validation of a Quantitative Core Shell-Based LC Separation for the Evaluation of Silymarin Variability and Associated Antioxidant Activity of Pakistani Ecotypes of Milk Thistle (Silybum Marianum L.)
Molecules 2018, 23(4), 904; https://doi.org/10.3390/molecules23040904
Received: 21 February 2018 / Revised: 6 April 2018 / Accepted: 13 April 2018 / Published: 14 April 2018
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Abstract
Fruits of Silybum marianum (L.) Gaernt are the main source of taxifolin derived flavonolignans. Together, these molecules constitute a mixture called silymarin with many useful applications for cosmetic and pharmaceutic industries. Here, a validated method for the separation of the silymarin constituents has
[...] Read more.
Fruits of Silybum marianum (L.) Gaernt are the main source of taxifolin derived flavonolignans. Together, these molecules constitute a mixture called silymarin with many useful applications for cosmetic and pharmaceutic industries. Here, a validated method for the separation of the silymarin constituents has been developed to ensure precision and accuracy in their quantification. Each compound was separated with a high reproducibility. Precision and repeatability of the quantification method were validated according to the AOAC recommendations. The method was then applied to study the natural variability of wild accessions of S. marianum. Analysis of the variation in the fruits composition of these 12 accessions from Pakistan evidenced a huge natural diversity. Correlation analysis suggested a synergistic action of the different flavonolignans to reach the maximal antioxidant activity, as determined by cupric ion reducing antioxidant capacity (CUPRAC) and ferric reducing antioxidant power (FRAP) assays. Principal component analysis (PCA) separated the 12 accessions into three distinct groups that were differing from their silymarin contents, whereas hierarchical clustering analysis (HCA) evidenced strong variations in their silymarin composition, leading to the identification of new silybin-rich chemotypes. These results proved that the present method allows for an efficient separation and quantification of the main flavonolignans with potent antioxidant activities. Full article
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Open AccessArticle New Findings in Prunus padus L. Fruits as a Source of Natural Compounds: Characterization of Metabolite Profiles and Preliminary Evaluation of Antioxidant Activity
Molecules 2018, 23(4), 725; https://doi.org/10.3390/molecules23040725
Received: 23 February 2018 / Revised: 14 March 2018 / Accepted: 21 March 2018 / Published: 22 March 2018
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Abstract
European bird cherry (Prunus padus L.) has been known since the Middle Ages for its medical/food use and high health-promoting value. This study aimed to assess the potential of these fruits as a source of bioactive compounds through the characterization of its
[...] Read more.
European bird cherry (Prunus padus L.) has been known since the Middle Ages for its medical/food use and high health-promoting value. This study aimed to assess the potential of these fruits as a source of bioactive compounds through the characterization of its physicochemical traits, nutraceutical properties, phytochemical composition via HPLC fingerprint, and antioxidant capacity. Fully ripened fruits of Prunus padus L. (Colorata cv) were collected in mid-July 2017 in Chieri, north-western Italy. The TPC (194.22 ± 32.83 mgGAE/100 gFW) and TAC (147.42 ± 0.58 mgC3G/100 gFW) values were obtained from the analyzed extracts. The most important phytochemical class was organic acids (48.62 ± 2.31%), followed by polyphenols (35.34 ± 1.80%), monoterpenes (9.36 ± 0.64%), and vitamin C (6.68 ± 0.22%). In this research the most important flavonols selected as marker were quercitrin (16.37 ± 3.51 mg/100 gFW) and quercetin (11.86 ± 2.36 mg/100 gFW). Data were reported based on fresh weight. Moreover, fresh fruits showed a mean antioxidant activity value of 17.78 ± 0.84 mmol Fe2+·kg−1. Even though the seeds and leaves contain cyanogenic glycosides, this study showed that these fruits could be a natural source of bioactive compounds with high antioxidant properties, due to the contents of organic and phenolic acids, catechins, and a synergetic effect of vitamin C and flavonoids. Full article
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Open AccessCommunication Development and Validation of a HPLC-UV Method for Extraction Optimization and Biological Evaluation of Hot-Water and Ethanolic Extracts of Dendropanax morbifera Leaves
Molecules 2018, 23(3), 650; https://doi.org/10.3390/molecules23030650
Received: 22 February 2018 / Revised: 9 March 2018 / Accepted: 12 March 2018 / Published: 13 March 2018
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Abstract
Dendropanax morbifera Leveille (Araliaceae) has been used in traditional oriental remedies for cancer, inflammation, diabetes, and thrombosis. However, a validated analytical method, standardization, and optimization of extraction conditions with respect to biological activity have not been reported. In this study, a simple and
[...] Read more.
Dendropanax morbifera Leveille (Araliaceae) has been used in traditional oriental remedies for cancer, inflammation, diabetes, and thrombosis. However, a validated analytical method, standardization, and optimization of extraction conditions with respect to biological activity have not been reported. In this study, a simple and validated HPLC method for identifying and quantifying active substances in D. morbifera was developed. Hot water and ethanolic D. morbifera leaf extracts from different production regions were prepared and evaluated with regard to their chemical compositions and biological activities. The contents of active compounds such as rutin and chlorogenic acid were determined in four samples collected from different regions. The 80% ethanolic extract showed the best antioxidant activity, phenolic content, reducing power, and xanthine oxidase (XO) inhibitory activity. The validated HPLC method confirmed the presence of chlorogenic acid and rutin in D. morbifera leaf extracts. The antioxidant and XO inhibitory activity of D. morbifera extract could be attributed to the marker compounds. Collectively, these results suggest that D. morbifera leaves could be beneficial for the treatment or prevention of hyperuricemia-related disease, and the validated HPLC method could be a useful tool for the quality control of food or drug formulations containing D. morbifera. Full article
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Open AccessArticle Comparison of Multiple Bioactive Constituents in Different Parts of Eucommia ulmoides Based on UFLC-QTRAP-MS/MS Combined with PCA
Molecules 2018, 23(3), 643; https://doi.org/10.3390/molecules23030643
Received: 20 January 2018 / Revised: 21 February 2018 / Accepted: 9 March 2018 / Published: 13 March 2018
Cited by 1 | PDF Full-text (1241 KB) | HTML Full-text | XML Full-text | Supplementary Files
Abstract
Eucommia ulmoides Oilv. (EU), also called Du-zhong, is a classical traditional Chinese medicine. Its bark, leaf, and male flower are all used for medicinal purposes, called Eucommiae Cortex (EC), Eucommiae Folium (EF), and Eucommiae Flos Male (EFM). In order to study the difference
[...] Read more.
Eucommia ulmoides Oilv. (EU), also called Du-zhong, is a classical traditional Chinese medicine. Its bark, leaf, and male flower are all used for medicinal purposes, called Eucommiae Cortex (EC), Eucommiae Folium (EF), and Eucommiae Flos Male (EFM). In order to study the difference in synthesis and the accumulation of metabolites in different parts of EU, a reliable method based on ultra-fast liquid chromatography tandem triple quadrupole mass spectrometry (UFLC-QTRAP-MS/MS) was developed for the simultaneous determination of a total of 21 constituents, including two lignans, 6 iridoids, 6 penylpropanoids, 6 flavonoids, and one phenol in the samples (EC, EF, and EFM). Furthermore, principal component analysis (PCA) was performed to evaluate and classify the samples according to the contents of these 21 constituents. All of the results demonstrated that the chemical compositions in EC, EF, and EFM were significantly different and the differential constituents (i.e., aucubin, geniposidic acid, chlorogenic acid, pinoresinol-di-O-β-d-glucopyranoside, geniposide, cryptochlorogenic acid, rutin, and quercetin) were remarkably associated with sample classifications. The research will provide the basic information for revealing the laws of metabolite accumulation in EC, EF, and EFM from the same origin. Full article
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Open AccessArticle Quality Evaluation of Apocyni Veneti Folium from Different Habitats and Commercial Herbs Based on Simultaneous Determination of Multiple Bioactive Constituents Combined with Multivariate Statistical Analysis
Molecules 2018, 23(3), 573; https://doi.org/10.3390/molecules23030573
Received: 29 January 2018 / Revised: 20 February 2018 / Accepted: 1 March 2018 / Published: 3 March 2018
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Abstract
Apocyni Veneti Folium (AVF) is a kind of staple traditional Chinese medicine with vast clinical consumption because of its positive effects. However, due to the habitats and adulterants, its quality is uneven. To control the quality of this medicinal herb, in this study,
[...] Read more.
Apocyni Veneti Folium (AVF) is a kind of staple traditional Chinese medicine with vast clinical consumption because of its positive effects. However, due to the habitats and adulterants, its quality is uneven. To control the quality of this medicinal herb, in this study, the quality of AVF was evaluated based on simultaneous determination of multiple bioactive constituents combined with multivariate statistical analysis. A reliable method based on ultra-fast liquid chromatography tandem triple quadrupole mass spectrometry (UFLC-QTRAP-MS/MS) was developed for the simultaneous determination of a total of 43 constituents, including 15 flavonoids, 6 organic acids, 13 amino acids, and 9 nucleosides in 41 Luobumaye samples from different habitats and commercial herbs. Furthermore, according to the contents of these 43 constituents, principal component analysis (PCA) was employed to classify and distinguish between AVF and its adulterants, leaves of Poacynum hendersonii (PHF), and gray relational analysis (GRA) was performed to evaluate the quality of the samples. The proposed method was successfully applied to the comprehensive quality evaluation of AVF, and all results demonstrated that the quality of AVF was higher than the PHF. This study will provide comprehensive information necessary for the quality control of AVF. Full article
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Open AccessArticle Molecular and Functional Properties of Protein Fractions and Isolate from Cashew Nut (Anacardium occidentale L.)
Molecules 2018, 23(2), 393; https://doi.org/10.3390/molecules23020393
Received: 9 January 2018 / Revised: 30 January 2018 / Accepted: 31 January 2018 / Published: 12 February 2018
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Abstract
Some molecular and functional properties of albumin (83.6% protein), globulin (95.5% protein), glutelin (81.3% protein) as well as protein isolate (80.7% protein) from cashew nut were investigated. These proteins were subjected to molecular (circular dichroism, gel electrophoresis, scanning electron microscopy) and functional (solubility,
[...] Read more.
Some molecular and functional properties of albumin (83.6% protein), globulin (95.5% protein), glutelin (81.3% protein) as well as protein isolate (80.7% protein) from cashew nut were investigated. These proteins were subjected to molecular (circular dichroism, gel electrophoresis, scanning electron microscopy) and functional (solubility, emulsification, foaming, water/oil holding capacity) tests. Cashew nut proteins represent an abundant nutrient with well-balanced amino acid composition and could meet the requirements recommended by FAO/WHO. SDS-PAGE pattern indicated cashew nut proteins were mainly composed of a polypeptide with molecular weight (MW) of 53 kDa, which presented two bands with MW of 32 and 21 kDa under reducing conditions. The far-UV CD spectra indicated that cashew proteins were rich in β-sheets. The surface hydrophobicity of the protein isolate was higher than that of the protein fractions. In pH 7.0, the solubility of protein fractions was above 70%, which was higher than protein isolate at any pH. Glutelin had the highest water/oil holding capacity and foaming properties. Protein isolate displayed better emulsifying properties than protein fractions. In summary, cashew nut kernel proteins have potential as valuable nutrition sources and could be used effectively in the food industry. Full article
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Planned Papers

The below list represents only planned manuscripts. Some of these manuscripts have not been received by the Editorial Office yet. Papers submitted to MDPI journals are subject to peer-review.

Title: The way to ultrafast, high-throughput enantioseparations of bioactive compounds in liquid and supercritical fluid chromatography
Article type: Review
Author: Prof. Alberto Cavazzini (University of Ferrara, Italy)
Abstract:Until less than 10 years ago, chiral separations were carried out with columns packed with 5 of 3 μm fully porous particles (FPPs). Times required to risolve enantiomeric mixtures were routinely larger than 30 minutes or so. Pushed especially by stringent requirements from medicinal and pharmaceutical industries, during the last years the field of chiral separations by liquid chromatography has undergone a true revolution.
With the purpose of developing ever faster and efficient method of separations, indeed, very efficient particle formats, such as superficially porous particles (SPPs) or sub-2μm FPPs, have been functionalized with chiral selectors and employed in ultrafast applications. Thanks to the use of short column (1-2 cm long), packed with these new generation chiral stationary phases (CSPs), operated at very high flow rates (5-8 mL/min), resolution of racemates could be accomplished in very short time, in many cases smaller than 1 sec. in normal-, reversed-phase and HILIC conditions.
Additionally, these CSPs have been found to be extremely promising also to carry out high-throughput separations under supercritical fluid chromatography (SFC) conditions.
In this manuscript, we will review the most important results that have been recently achieved in terms of ultrafast, high-throughput enantioseparations both in liquid and supercritical fluid chromatography with particular attention to the very important field of bioactive chiral compounds. Attention will be focused not only on the latest introduced CSPs and their applications, but also on instrumental modifications which are required in some cases in order to fully exploit the intrinsic potential of new generation chiral columns.

Title: Variation in the carotenoid composition and in their bioaccessibility from Delica (Cucurbita maxima) and Violina (Cucurbita moschata) pumpkins with food processing
Article type: Article
Author: Prof. Dr. Nicola Marchetti(University of Ferrara, Italy)
Abstract:In the last years, a great attention has been dedicated to the consumption of fresh vegetables and fruits since they have antioxidant and anticarcinogenic properties. Carotenoids are a widespread group of fat soluble pigments and their major nutritional importance comes from their pro–vitamin A activity.
In this study, two different cultivars of pumpkin (Cucurbita maxima, also named ‘Delica’ and Cucurbita moschata, known as ‘Violina’) from southern Po Delta area were studied in terms of carotenoids content and the influence of food processing on compositional changes and carotenoids bioaccessibility.
Qualitative investigation and quantitative determination have been performed on sample extracts by C3o HPLC with UV-Vis detector. In agreement with literature studies on selectivity, two main classes of compounds can be separated: early eluted epoxy– and hydroxy–carotenoids; more retained hydrocarbon–derivatives or carotenes. Major qualitative differences are visible in the chromatographic profiles: C. maxima presented 10 well separated peaks while it was smaller for C. moschata (6 peaks). The identification of chromatographic bands was tentatively obtained by means of (i) the chromatographic parameters, (ii) the UV–Vis spectra and relative maxima intensities, (iii) MS/MS spectra. Quantification of target carotenoids was performed with external calibration through analytical standards. The concentration of lutein and β-carotene was higher in C. maxima than in the other variety C. moschata.
Carotenoids are susceptible to degradation (isomerization and oxidation) during food processing (i.e., cooking) and the concentration of lutein and β-carotene were monitored in oven–cooked and steam– cooked pumpkins. Steam cooking process resulted to be superior to the other in terms of limiting the loss of carotenoids. A complete functional profile of pumpkins as a source of carotenoids was gained with the evaluation of their in vitro bioaccessibility and their bioavailability after intake during human digestion. Bioaccessibility of lutein and β-carotene were estimated by in vitro static digestion model that involves salivary, gastric and duodenal phases. Bioaccessibility values progressively increase from salivary to duodenal phase for both pumpkin variety and cooking method. At the duodenal stage bioaccessibility of lutein was always three times lower than β-carotene and no specific differences in the bioaccessibility were evidenced between the two cultivars for all the three digestion phases.
Keywords: carotenoids, pumpkins, HPLC – DAD, C30 column, bioaccessibility

Title: New Findings in Prunus padus l. Fruits as Source of Natural Compounds: Characterization of Metabolite Profiles and Antioxidant Activity
Article type: Article
Authors: Donno D., Mellano M.G., De Biaggi M., Riondato I., Rakotoniaina E.N., Beccaro G.L.
Affiliation: Università degli Studi di Torino, Italy
Abstract:In recent years, wild food plants have become very attractive to the food industry, prompting their use as replacements for synthetic chemicals and nutraceuticals, but neglected and underutilized natural food resources are suffering from less attention and research, and their nutritional, economic and socio-cultural potentials are not fully exploited. A global trend for the revival of interest in the use of traditional plants in daily menu has been observed. European bird cherry (Prunus padus L.) has been known since Middle Age for its medical/food use and high health-promoting value. This study aimed to assess the potential of these fruits as potential source of bioactive compounds by characterizing its physicochemical traits, nutraceutical properties, phytochemical composition by HPLC fingerprint, and antioxidant capacity. Fully ripened fruits (0.5 kg for each biological replication) of a cultivated genotype of Prunus padus L. (Colorata cv) were collected in the in mid-July 2017, in Chieri (45°1’0”N, 7°49’0”E, at 305 m A.S.L.), Piedmont (north-western Italy), in a germplasm repository of the Department of Agricultural, Forest and Food Sciences, University of Turin (voucher specimens were deposited). In this research the used methods allowed an accurate and rapid measurement of total monomeric anthocyanins and total polyphenolic content. The TPC (194.22±32.83 mgGAE/100gFW) and TAC (147.42±0.58 mgC3G/100gFW) values were obtained from the analyzed extracts. The most important phytochemical class was organic acids (48.62±2.31%), followed by polyphenols (35.34±1.80%), monoterpenes (9.36±0.64%), and vitamin C (6.68±0.22%). In this research the most important flavonols selected as marker were quercitrin (16.37±3.51 mg/100 gFW) and quercetin (11.86 ±2.36 mg/100 gFW), followed by hyperoside (7.38±0.41 mg/100 gFW) and rutin (2.67 ±1.02 mg/100 gFW). Moreover, the presence of cinnamic acids, in particular chlorogenic acid (10.48±0.28 mg/100 gFW), may be important when fruits are processed, as these compounds are considered a preferential substrate for the catecholase activity of polyphenol oxidase. Bird cherry fruits showed a total vitamin C content (76.07±13.34 mg/100 gFW) similar to the most common fruits, as kiwifruit (74.56±9.84 mg/100 gFW) and orange (71.12±1.96 mg/100 gFW). Data were reported based on fresh weight. Moreover, fresh fruits showed a mean antioxidant activity value of 17.78±0.84 mmol Fe2+•kg−1. Despite the seeds and leaves contain cyanogenic glycosides, this study showed that these fruits could be a potential natural source of bioactive compounds with high antioxidant properties, due to the contents of organic and phenolic acids, catechins, and a synergetic effect of vitamin C and flavonoids.
Keywords: bird cherry, fruit healthy properties, biodiversity, phytochemicals, traditional food, chromatographic fingerprinting, antioxidants

Title: Chromatographic strategies for separation of bioactive compounds in food matrices
Article type: Review
Author: Prof. Dr. Anna Laura Capriotti (University of Rome, Italy)

Title: Tracing the Thermal History of Seafood Products Through Lysophospholipid Analysis by Hydrophilic Interaction Liquid Chromatography-Electrospray Ionization and Fourier-Transform Mass Spectrometry
Article type: Article
Authors: Dr. Ilario Losito, Dr. Laura Facchini, Dr. Rosa Catucci and Prof. Tommaso Cataldi and Francesco Palmisano (University of Bari "Aldo Moro", Italy)

Title: A toolbox of methods for characterization of phospholipids and their oxidized derivatives in food and biological samples
Article type: Review
Authors: Dr. Agnieszka Bartoszek

Title: ODAP content in Lathyrus sativus (grass pea): implementation and validation of a simple and fast LC-MS/MS method
Article type: Article
Authors: Dr. Andreia Bento da Silva (Food Functionality and Bioactives Lab, Portugal)

Title: Chiral Separation of Indapamide on Polysaccharide Stationary Phase
Article type: Article
Authors:Tomasz Baczek

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