Luca Rastrelli | University of Salerno (original) (raw)

Papers by Luca Rastrelli

Research paper thumbnail of Ultrasound assisted dispersive liquid-liquid microextraction for fast and accurate analysis of chloramphenicol in honey

Food Research International, 2019

A sensitive and fast ultrasound-assisted dispersive liquid-liquid microextraction procedure combi... more A sensitive and fast ultrasound-assisted dispersive liquid-liquid microextraction procedure combined with ion mobility spectrometry has been developed for the simultaneous extraction and determination of bendiocarb and azinphos-ethyl. Experimental parameters affecting the analytical performance of the method were optimized: type and volume of extraction solvent (chloroform, 150 µL), pH (9.0), type and volume of buffer (ammonium buffer pH = 9.0, 4.5 mL) and extraction time (3.0 min). Under optimum conditions, the linearity was found to be in the range of 2-40 and 6-100 ng/mL and the limits of detection (LOD) were 1.04 and 1.31 ng/mL for bendiocarb and azinphos-ethyl, respectively. The method was successfully validated for the analysis of bendiocarb and azinphos-ethyl in different samples such as waters, soil, food and beverage samples.

Research paper thumbnail of Assessment of mycotoxins co‐occurrence in Italian dried figs and in dried figs‐based products

Journal of Food Safety, Sep 10, 2018

The possible contamination by aflatoxins (AFs), ochratoxin A (OTA), fumonisin B 1 (FB 1), fusaric... more The possible contamination by aflatoxins (AFs), ochratoxin A (OTA), fumonisin B 1 (FB 1), fusaric acid (FA), and beauvericin (BEA), was investigated in 55 samples of dried figs and dried figs-based products purchased from the South Italy (Calabria) market. A total of 41 samples showed contamination by at least one of the mycotoxins investigated. Aflatoxin B 1 was found in six samples (0.19-8.41 μg/kg) total aflatoxins were found in 13 samples (0.5-17.12 μg/kg), OTA was found in 21 samples (<LOQ-158.58 μg/kg), FB 1 was found in eight samples (153.81-5,412.96 μg/kg), BEA was found in 12 samples (<LOQ-5,708.49 μg/kg), and FA was found in 28 samples (<LOQ-74,520.20 μg/kg). The analyzed samples were contaminated with one (41.8%), two (7.3%), three (5.5%), four (10.9%), and five (5.5%) mycotoxins. To the best of our knowledge, the incidence of contamination by FA and BEA has been shown for the first time in dried figs.

Research paper thumbnail of Determination of mycotoxins in beer by multi heart-cutting two-dimensional liquid chromatography tandem mass spectrometry method

Food Chemistry, Jul 1, 2020

This is a PDF file of an article that has undergone enhancements after acceptance, such as the ad... more This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover page and metadata, and formatting for readability, but it is not yet the definitive version of record. This version will undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing this version to give early visibility of the article. Please note that, during the production process, errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

Research paper thumbnail of Specialized metabolite profiling of different Glycyrrhiza glabra organs by untargeted UHPLC-HRMS

Industrial Crops and Products, 2021

Abstract Calabrian licorice (roots of G. glabra var. typica), PDO certified, is one of the most v... more Abstract Calabrian licorice (roots of G. glabra var. typica), PDO certified, is one of the most valuable commercial within Glycyrrhiza species. Specialized metabolites profiling of below and aboveground parts of PDO Calabrian G. glabra was established by untargeted UHPLC-HRMS either to elucidate their distinctive accumulation among tissues and to gain insight about the chemical composition of leaves and exudate, also to provide fingerprints for PDO products authentication. Roots showed the typical profile of G. glabra, namely glabridin and prenylated phenolic compounds (erybacin B, kanzonol Y, mulberrofuran K isomers, 3-hydroxyglabrol and glabrol) were confirmed as useful species-specific markers for authenticity and traceability of Calabrian licorice. Aerial tissues contained exclusively phenolics compounds, with pinocembrin, prenylated flavanones (licoflavanone and glabranin) and dihydrostilbenes as distinctive metabolites accumulated in the leaf-exudates, and glycosylated flavonoids (isoquercitrin, astragalin and their malonyl derivatives) distributed solely in the inner leaf tissues and flowers. This comparative study provides insights on tissue-distribution of G. glabra specialized metabolites and paves the way for sustainable valorization of untapped resources and improves the economic value of supply licorice-chain.

Research paper thumbnail of Onion Peel: Turning a Food Waste into a Resource

Antioxidants, 2021

Food waste is a serious problem for food processing industries, especially when it represents a l... more Food waste is a serious problem for food processing industries, especially when it represents a loss of a valuable source of nutrients and phytochemicals. Increasing consumer demand for processed food poses the problem of minimizing waste by conversion into useful products. In this regard, onion (Allium cepa) waste consisting mainly of onion skin is rich in bioactive phenolic compounds. Here, we characterized the flavonoid profiles and biological activities of onion skin wastes of two traditional varieties with protected geographical indication (PGI), the red “Rossa di Tropea” and the coppery “Ramata di Montoro”, typically cultivated in a niche area in southern Italy. The phytochemical profiles of exhaustive extracts, characterized by ultra-high-performance liquid chromatography coupled with ultraviolet (UV) detection and high-resolution mass spectrometry, revealed that flavonols and anthocyanins were the characteristic metabolite classes of onion skins. Quercetin, quercetin glucosi...

Research paper thumbnail of Determination of Chloramphenicol in Honey Using Salting-Out Assisted Liquid-Liquid Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry and Validation According to 2002/657 European Commission Decision

Molecules, 2020

Honey is a natural food widely consumed due to its high content in nutrients and bioactive substa... more Honey is a natural food widely consumed due to its high content in nutrients and bioactive substances. In order to prevent hive infections, xenobiotics such as pesticides and antibiotics are commonly used. Chloramphenicol (CAP) is a broad-spectrum antibiotic used to treat honeybee larvae diseases. However, CAP has toxic and nondose-dependent effects in sensitive subjects; for this reason, its use has been prohibited in food-producing animals, such as the honeybee. In this study, we proposed a rapid, simple, and cheap analytical method, based on salting-out assisted liquid-liquid extraction coupled with UHPLC MS/MS detection for the accurate determination of CAP in honey to be used in routine analyses. The parameters that influence the extraction efficiency have been optimized using an experimental design in order to maximize the recovery of the analyte by reducing the matrix effects. Therefore, the developed method was internally validated according to the 2002/657/EC Decision guide...

Research paper thumbnail of Development of an Enriched Polyphenol (Natural Antioxidant) Extract from Orange Juice (Citrus sinensis) by Adsorption on Macroporous Resins

Journal of Food Quality, 2020

Orange (Citrus sinensis) juice contains a high amount of antioxidant compounds, such as polypheno... more Orange (Citrus sinensis) juice contains a high amount of antioxidant compounds, such as polyphenols and vitamins. The aim of this work was to develop an adsorption procedure for the quantitative recovery of polyphenols from fresh orange juice. Different macroporous resins have been selected to evaluate their affinity for phenolic compound in order to purify the antioxidant compounds from the orange juice. The main compounds of orange juice were firstly characterized using an UPLC-UV-HRMS to define the metabolite profile, and subsequently three different types of adsorbent (XAD-2, XAD-4, and XAD-16N) were tested to concentrate these bioactive compounds. The time of contact was selected based on kinetic studies, and subsequently the adsorption and elution conditions were optimized in order to maximize the recovery of phenolic compounds to obtain an extract rich of bioactive compounds. Lastly, antioxidant capacity of the orange juice extract of selected macroporous resin, obtained unde...

Research paper thumbnail of Phenolic Derivatives from the Leaves of Martinella Obovata (Bignoniaceae)

Natural Product Communications, 2011

A new phenolic derivative, 4-methoxyphenol 1-O-β-D-apiofuranosyl-(1→6)-O--D-glucopyranoside (1),... more A new phenolic derivative, 4-methoxyphenol 1-O-β-D-apiofuranosyl-(1→6)-O--D-glucopyranoside (1), has been identified together with uncommon 3,4-dimethoxyphenol 1-O-β-D-apiofuranosyl-(1→6)-O--D-glucopyranoside (2) and 3-hydroxy, 4-methoxyphenol 1-O-β-Dapiofuranosyl-(1→6)-O--D-glucopyranoside (3) from the leaves of Martinella obovata (Kunth) Bureau & K. Schum., an Honduran species used in folk medicine for the treatment of eyes diseases. Verbascoside, isoverbascoside, leucoceptoside A, vitexin, isovitexin, luteolin 8-C-β-D-glucopiranoside and spireoside were also found. All structures were elucidated on the basis of mass spectrometry and 2D NMR techniques.

Research paper thumbnail of Magnoflorine and Phenolic Derivatives from the Leaves of Croton xalapensis L. (Euphorbiaceae)

Natural Product Communications, 2009

The alkaloid magnoflorine 1, has been isolated for the first time from Croton xalapensis (Euphorb... more The alkaloid magnoflorine 1, has been isolated for the first time from Croton xalapensis (Euphorbiaceae), in addition two phenylpropenols derivates, 3,4-dimethoxy-(E)-cinnamyl alcohol 2 and 3,4-dimethoxy-5-hydroxy-(E)-cinnamyl alcohol 3, 3,4,5-trimethoxycinnamic acid 4, gallic acid 5, methyl gallate 6 and 3,4-dihydroxybenzoic acid 7 have been also found; these compounds were identified by spectroscopic analysis particularly, 2D NMR and ESI-MS/MS techniques. The high concentration of magnoflorine, calculated with quantitative HPLC, of the aqueous extract, probably contributes to the remarkable medicinal properties of this plant. In addition this is the first phytochemical study on Croton xalapensis to be reported.

Research paper thumbnail of Response surface methodology to optimize supercritical carbon dioxide/co-solvent extraction of brown onion skin by-product as source of nutraceutical compounds

Food chemistry, Jan 15, 2018

Food industry produces a large amount of onion wastes. Due to the high amount of bioactive compou... more Food industry produces a large amount of onion wastes. Due to the high amount of bioactive compounds in onion by-products an idea for their reuse, could be use them as source of high-value functional and health ingredients. In this study, outer dry layers of coppery onion "Ramata di Montoro" were used as source of bioactive compounds. Firstly, the chemical profile of secondary metabolites of exhaustive extract, obtained by ultrasound assisted extraction was established by UHPLC-UV-HRMS/MS analysis. Subsequently, the supercritical fluid extraction was used as alternative and green method to recover flavonoids from onion skin. Main parameters such as pressure, temperature and composition of solvent modifier were optimized in order to improve the extraction efficiency of SFE technique, by using a response surface Box-Behnken design.

Research paper thumbnail of Characterisation of nutraceutical compounds from different parts of particular species of Citrus sinensis 'Ovale Calabrese' by UHPLC-UV-ESI-HRMS

Natural product research, Jan 23, 2018

Consumers are aware of diet causing health problems and therefore there is an increased demand fo... more Consumers are aware of diet causing health problems and therefore there is an increased demand for natural ingredients that are expected to be safe and health-promoting. Many of these compounds belong to the class of flavonoids and can be divided into these five groups: flavanones, flavones, flavonols, flavanols, isoflavones and anthocyanidins. Extracts from citrus fruits are usually used as functional ingredients for several products. The aim of this paper was to develop an UHPLC-UV-ESI-HRMS method to define the metabolite profile of different parts of citrus fruit, of a particular cultivar called 'Ovale Calabrese', and in its main by-products. The high resolution mass spectrometry analysis allowed the identification of 27 compounds belonging to the classes of flavonoids and terpenoids. The high contents of phytochemical compounds, reveal the potential use of the 'Ovale Calabrese' as a rich source of nutraceutical compounds.

Research paper thumbnail of Selective extraction of high-value phenolic compounds from distillation wastewater of basil (Ocimum basilicum L.) by pressurized liquid extraction

Electrophoresis, Jan 31, 2018

During the essential oil steam distillation from aromatic herbs, huge amounts of distillation was... more During the essential oil steam distillation from aromatic herbs, huge amounts of distillation wastewaters (DWWs) are generated. These by-products represent an exceptionally rich source of phenolic compounds such as rosmarinic acid (RA) and caffeic acid (CA). Herein, the alternative use of dried basil DWWs (dDWWs) to perform a selective extraction of RA and CA by pressurized liquid extraction (PLE) employing bio-based solvent was studied. To select the most suitable solvent for PLE, the theoretical modelling of Hansen solubility parameters (HSP) was carried out. This approach allows reducing the list of candidate to two solvents: ethanol and ethyl lactate. Due to the composition of the sample, mixtures of water with those solvents were also tested. An enriched PLE extract in RA (23.90 ± 2.06 mg/g extract) with an extraction efficiency of 75.89 ± 16.03% employing a water-ethanol mixture 25:75 (% v/v) at 50°C was obtained. In the case of CA, a PLE extract with 2.42 ± 0.04 mg/g extract,...

Research paper thumbnail of Occurrence of aflatoxin M1 in milk samples from Italy analysed by online-SPE UHPLC-MS/MS

Natural product research, Jan 17, 2017

The occurrence of aflatoxin M1 in 69 milk samples collected in a south region of Italy in 2016 wa... more The occurrence of aflatoxin M1 in 69 milk samples collected in a south region of Italy in 2016 was evaluated. The samples were analysed using an automated method based on online SPE coupled with UHPLC tandem mass spectrometry. After a salt induced liquid-liquid extraction with acetonitrile to remove protein from milk, the extract was diluted with water and analysed using an automated online SPE MS/MS method. Among the analysed samples no one had AFM1 higher than the legally allowable limits whereas 71.4% of the other analysed samples were above the LOD of the method. The highest contamination level of AFM1 was found in pasteurised milk (44.39 ng kg-1). The results show the worrying and widespread of AFM1 contamination, highlighting the necessity of monitoring studies in order to evaluate the reduction of the maximum legal limit.

Research paper thumbnail of Rapid and automated on-line solid phase extraction HPLC-MS/MS with peak focusing for the determination of ochratoxin A in wine samples

Food chemistry, 2018

This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS m... more This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS method for the automatic pre-concentration, clean up and sensitive determination of OTA in wine. The amount of OTA contained in 100μL of sample (pH≅5.5) was retained and concentrated on an Oasis MAX SPE cartridge. After a washing step to remove matrix interferents, the analyte was eluted in back-flush mode and the eluent from the SPE column was diluted through a mixing Tee, using an aqueous solution before the chromatographic separation achieved on a monolithic column. The developed method has been validated according to EU regulation N. 519/2014 and applied for the analysis of 41 red and 17 white wines. The developed method features minimal sample handling, low solvent consumption, high sample throughput, low analysis cost and provides an accurate and highly selective results.

Research paper thumbnail of Focusing and non-focusing modulation strategies for the improvement of on-line two-dimensional hydrophilic interaction chromatography × reversed phase profiling of complex food samples

Analytica chimica acta, Jan 8, 2017

Comprehensive two-dimensional liquid chromatography (LC × LC) is ever gaining interest in food an... more Comprehensive two-dimensional liquid chromatography (LC × LC) is ever gaining interest in food analysis, as often, food-related samples are too complex to be analyzed through one-dimensional approaches. The use of hydrophilic interaction chromatography (HILIC) combined with reversed phase (RP) separations has already been demonstrated as a very orthogonal combination, which allows attaining increased resolving power. However, this coupling encompasses different analytical challenges, mainly related to the important solvent strength mismatch between the two dimensions, besides those common to every LC × LC method. In the present contribution, different strategies are proposed and compared to further increase HILIC × RP method performance for the analysis of complex food samples, using licorice as a model sample. The influence of different parameters in non-focusing modulation methods based on sampling loops, as well as under focusing modulation, through the use of trapping columns in...

Research paper thumbnail of Oil distillation wastewaters from aromatic herbs as new natural source of antioxidant compounds

Food research international (Ottawa, Ont.), 2017

Distillation wastewaters (DWWs) are generated during the essential oil steam distillation from ar... more Distillation wastewaters (DWWs) are generated during the essential oil steam distillation from aromatic herbs. Despite of growing interest on novel source of natural antioxidant compounds as food additives, studies on DWWs are scarse. Herein, the potential of DWWs produced by the distillation of packaged fresh basil, rosemary and sage wastes was evaluated by chemical and antioxidant characterization. HPLC-DAD-HRMS profiling revealed that DWWs contain water-soluble phenolic compounds, mainly caffeic acid derivatives and flavonoid glycosides, with rosmarinic acid (RA) as predominant components (29-135mg/100mL). DWWs demonstrated high levels of total phenolic compounds (TPC, 152-443mg GAE/100mL) and strong antioxidant capacities, in ORAC, DPPH and ABTS assays (1101-4720, 635-4244 and 571-3145μmol TE/100mL, respectively). Highly significant correlations of TEAC values with TPC and RA contents revealed that phenolic compounds and high RA content were responsible of DWWs antioxidant prope...

Research paper thumbnail of Metabolite profiling of licorice (Glycyrrhiza glabra) from different locations using comprehensive two-dimensional liquid chromatography coupled to diode array and tandem mass spectrometry detection

Analytica Chimica Acta, 2016

profiling of licorice (Glycyrrhiza glabra) from different locations using comprehensive two-dimen... more profiling of licorice (Glycyrrhiza glabra) from different locations using comprehensive two-dimensional liquid chromatography coupled to diode array and tandem mass spectrometry detection,

Research paper thumbnail of A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography–tandem mass spectrometry

Analytical and Bioanalytical Chemistry, 2015

According to current demands and future perspectives in food safety, this study reports a fast an... more According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30 %) at 110°C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103 %) and repeatability (RSD<8, n=3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling highthroughput analysis and highly accurate and precise results.

Research paper thumbnail of Fragmentation pathways of polycyclic polyisoprenylated benzophenones and degradation profile of nemorosone by multiple-stage tandem mass spectrometry

Journal of the American Society for Mass Spectrometry, 2009

Research paper thumbnail of New Lignans from the Roots of Valeriana prionophylla with Antioxidative and Vasorelaxant Activities

Journal of Natural Products, 2004

Two new 7,9&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;a... more Two new 7,9&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;:7&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;,9-diepoxylignan glycosides have been isolated from the roots of Valeriana prionophylla. Their structures have been established on the basis of 1D and 2D NMR experiments as prinsepiol-4-O-beta-D-glucopyranoside (1) and fraxiresinol-4&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;-O-beta-D-glucopyranoside (2). In addition, 8-hydroxypinoresinol-4&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;-O-beta-d-glucopyranoside (3), 8-hydroxypinoresinol (4), prinsepiol (5), and chlorogenic acid were isolated. Compounds 1, 3, 4, and 5 were evaluated for their antioxidative properties in Trolox equivalent antioxidant activity (TEAC) and chemiluminescence (CL) assays. The same compounds were tested for their vascular activity in rat aorta rings. The aglycones 4 and 5 displayed powerful antioxidant activity; in addition, aglycone 4 showed a higher vasorelaxant activity than compounds 1, 3, and 5.

Research paper thumbnail of Ultrasound assisted dispersive liquid-liquid microextraction for fast and accurate analysis of chloramphenicol in honey

Food Research International, 2019

A sensitive and fast ultrasound-assisted dispersive liquid-liquid microextraction procedure combi... more A sensitive and fast ultrasound-assisted dispersive liquid-liquid microextraction procedure combined with ion mobility spectrometry has been developed for the simultaneous extraction and determination of bendiocarb and azinphos-ethyl. Experimental parameters affecting the analytical performance of the method were optimized: type and volume of extraction solvent (chloroform, 150 µL), pH (9.0), type and volume of buffer (ammonium buffer pH = 9.0, 4.5 mL) and extraction time (3.0 min). Under optimum conditions, the linearity was found to be in the range of 2-40 and 6-100 ng/mL and the limits of detection (LOD) were 1.04 and 1.31 ng/mL for bendiocarb and azinphos-ethyl, respectively. The method was successfully validated for the analysis of bendiocarb and azinphos-ethyl in different samples such as waters, soil, food and beverage samples.

Research paper thumbnail of Assessment of mycotoxins co‐occurrence in Italian dried figs and in dried figs‐based products

Journal of Food Safety, Sep 10, 2018

The possible contamination by aflatoxins (AFs), ochratoxin A (OTA), fumonisin B 1 (FB 1), fusaric... more The possible contamination by aflatoxins (AFs), ochratoxin A (OTA), fumonisin B 1 (FB 1), fusaric acid (FA), and beauvericin (BEA), was investigated in 55 samples of dried figs and dried figs-based products purchased from the South Italy (Calabria) market. A total of 41 samples showed contamination by at least one of the mycotoxins investigated. Aflatoxin B 1 was found in six samples (0.19-8.41 μg/kg) total aflatoxins were found in 13 samples (0.5-17.12 μg/kg), OTA was found in 21 samples (<LOQ-158.58 μg/kg), FB 1 was found in eight samples (153.81-5,412.96 μg/kg), BEA was found in 12 samples (<LOQ-5,708.49 μg/kg), and FA was found in 28 samples (<LOQ-74,520.20 μg/kg). The analyzed samples were contaminated with one (41.8%), two (7.3%), three (5.5%), four (10.9%), and five (5.5%) mycotoxins. To the best of our knowledge, the incidence of contamination by FA and BEA has been shown for the first time in dried figs.

Research paper thumbnail of Determination of mycotoxins in beer by multi heart-cutting two-dimensional liquid chromatography tandem mass spectrometry method

Food Chemistry, Jul 1, 2020

This is a PDF file of an article that has undergone enhancements after acceptance, such as the ad... more This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover page and metadata, and formatting for readability, but it is not yet the definitive version of record. This version will undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing this version to give early visibility of the article. Please note that, during the production process, errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain.

Research paper thumbnail of Specialized metabolite profiling of different Glycyrrhiza glabra organs by untargeted UHPLC-HRMS

Industrial Crops and Products, 2021

Abstract Calabrian licorice (roots of G. glabra var. typica), PDO certified, is one of the most v... more Abstract Calabrian licorice (roots of G. glabra var. typica), PDO certified, is one of the most valuable commercial within Glycyrrhiza species. Specialized metabolites profiling of below and aboveground parts of PDO Calabrian G. glabra was established by untargeted UHPLC-HRMS either to elucidate their distinctive accumulation among tissues and to gain insight about the chemical composition of leaves and exudate, also to provide fingerprints for PDO products authentication. Roots showed the typical profile of G. glabra, namely glabridin and prenylated phenolic compounds (erybacin B, kanzonol Y, mulberrofuran K isomers, 3-hydroxyglabrol and glabrol) were confirmed as useful species-specific markers for authenticity and traceability of Calabrian licorice. Aerial tissues contained exclusively phenolics compounds, with pinocembrin, prenylated flavanones (licoflavanone and glabranin) and dihydrostilbenes as distinctive metabolites accumulated in the leaf-exudates, and glycosylated flavonoids (isoquercitrin, astragalin and their malonyl derivatives) distributed solely in the inner leaf tissues and flowers. This comparative study provides insights on tissue-distribution of G. glabra specialized metabolites and paves the way for sustainable valorization of untapped resources and improves the economic value of supply licorice-chain.

Research paper thumbnail of Onion Peel: Turning a Food Waste into a Resource

Antioxidants, 2021

Food waste is a serious problem for food processing industries, especially when it represents a l... more Food waste is a serious problem for food processing industries, especially when it represents a loss of a valuable source of nutrients and phytochemicals. Increasing consumer demand for processed food poses the problem of minimizing waste by conversion into useful products. In this regard, onion (Allium cepa) waste consisting mainly of onion skin is rich in bioactive phenolic compounds. Here, we characterized the flavonoid profiles and biological activities of onion skin wastes of two traditional varieties with protected geographical indication (PGI), the red “Rossa di Tropea” and the coppery “Ramata di Montoro”, typically cultivated in a niche area in southern Italy. The phytochemical profiles of exhaustive extracts, characterized by ultra-high-performance liquid chromatography coupled with ultraviolet (UV) detection and high-resolution mass spectrometry, revealed that flavonols and anthocyanins were the characteristic metabolite classes of onion skins. Quercetin, quercetin glucosi...

Research paper thumbnail of Determination of Chloramphenicol in Honey Using Salting-Out Assisted Liquid-Liquid Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry and Validation According to 2002/657 European Commission Decision

Molecules, 2020

Honey is a natural food widely consumed due to its high content in nutrients and bioactive substa... more Honey is a natural food widely consumed due to its high content in nutrients and bioactive substances. In order to prevent hive infections, xenobiotics such as pesticides and antibiotics are commonly used. Chloramphenicol (CAP) is a broad-spectrum antibiotic used to treat honeybee larvae diseases. However, CAP has toxic and nondose-dependent effects in sensitive subjects; for this reason, its use has been prohibited in food-producing animals, such as the honeybee. In this study, we proposed a rapid, simple, and cheap analytical method, based on salting-out assisted liquid-liquid extraction coupled with UHPLC MS/MS detection for the accurate determination of CAP in honey to be used in routine analyses. The parameters that influence the extraction efficiency have been optimized using an experimental design in order to maximize the recovery of the analyte by reducing the matrix effects. Therefore, the developed method was internally validated according to the 2002/657/EC Decision guide...

Research paper thumbnail of Development of an Enriched Polyphenol (Natural Antioxidant) Extract from Orange Juice (Citrus sinensis) by Adsorption on Macroporous Resins

Journal of Food Quality, 2020

Orange (Citrus sinensis) juice contains a high amount of antioxidant compounds, such as polypheno... more Orange (Citrus sinensis) juice contains a high amount of antioxidant compounds, such as polyphenols and vitamins. The aim of this work was to develop an adsorption procedure for the quantitative recovery of polyphenols from fresh orange juice. Different macroporous resins have been selected to evaluate their affinity for phenolic compound in order to purify the antioxidant compounds from the orange juice. The main compounds of orange juice were firstly characterized using an UPLC-UV-HRMS to define the metabolite profile, and subsequently three different types of adsorbent (XAD-2, XAD-4, and XAD-16N) were tested to concentrate these bioactive compounds. The time of contact was selected based on kinetic studies, and subsequently the adsorption and elution conditions were optimized in order to maximize the recovery of phenolic compounds to obtain an extract rich of bioactive compounds. Lastly, antioxidant capacity of the orange juice extract of selected macroporous resin, obtained unde...

Research paper thumbnail of Phenolic Derivatives from the Leaves of Martinella Obovata (Bignoniaceae)

Natural Product Communications, 2011

A new phenolic derivative, 4-methoxyphenol 1-O-β-D-apiofuranosyl-(1→6)-O--D-glucopyranoside (1),... more A new phenolic derivative, 4-methoxyphenol 1-O-β-D-apiofuranosyl-(1→6)-O--D-glucopyranoside (1), has been identified together with uncommon 3,4-dimethoxyphenol 1-O-β-D-apiofuranosyl-(1→6)-O--D-glucopyranoside (2) and 3-hydroxy, 4-methoxyphenol 1-O-β-Dapiofuranosyl-(1→6)-O--D-glucopyranoside (3) from the leaves of Martinella obovata (Kunth) Bureau & K. Schum., an Honduran species used in folk medicine for the treatment of eyes diseases. Verbascoside, isoverbascoside, leucoceptoside A, vitexin, isovitexin, luteolin 8-C-β-D-glucopiranoside and spireoside were also found. All structures were elucidated on the basis of mass spectrometry and 2D NMR techniques.

Research paper thumbnail of Magnoflorine and Phenolic Derivatives from the Leaves of Croton xalapensis L. (Euphorbiaceae)

Natural Product Communications, 2009

The alkaloid magnoflorine 1, has been isolated for the first time from Croton xalapensis (Euphorb... more The alkaloid magnoflorine 1, has been isolated for the first time from Croton xalapensis (Euphorbiaceae), in addition two phenylpropenols derivates, 3,4-dimethoxy-(E)-cinnamyl alcohol 2 and 3,4-dimethoxy-5-hydroxy-(E)-cinnamyl alcohol 3, 3,4,5-trimethoxycinnamic acid 4, gallic acid 5, methyl gallate 6 and 3,4-dihydroxybenzoic acid 7 have been also found; these compounds were identified by spectroscopic analysis particularly, 2D NMR and ESI-MS/MS techniques. The high concentration of magnoflorine, calculated with quantitative HPLC, of the aqueous extract, probably contributes to the remarkable medicinal properties of this plant. In addition this is the first phytochemical study on Croton xalapensis to be reported.

Research paper thumbnail of Response surface methodology to optimize supercritical carbon dioxide/co-solvent extraction of brown onion skin by-product as source of nutraceutical compounds

Food chemistry, Jan 15, 2018

Food industry produces a large amount of onion wastes. Due to the high amount of bioactive compou... more Food industry produces a large amount of onion wastes. Due to the high amount of bioactive compounds in onion by-products an idea for their reuse, could be use them as source of high-value functional and health ingredients. In this study, outer dry layers of coppery onion "Ramata di Montoro" were used as source of bioactive compounds. Firstly, the chemical profile of secondary metabolites of exhaustive extract, obtained by ultrasound assisted extraction was established by UHPLC-UV-HRMS/MS analysis. Subsequently, the supercritical fluid extraction was used as alternative and green method to recover flavonoids from onion skin. Main parameters such as pressure, temperature and composition of solvent modifier were optimized in order to improve the extraction efficiency of SFE technique, by using a response surface Box-Behnken design.

Research paper thumbnail of Characterisation of nutraceutical compounds from different parts of particular species of Citrus sinensis 'Ovale Calabrese' by UHPLC-UV-ESI-HRMS

Natural product research, Jan 23, 2018

Consumers are aware of diet causing health problems and therefore there is an increased demand fo... more Consumers are aware of diet causing health problems and therefore there is an increased demand for natural ingredients that are expected to be safe and health-promoting. Many of these compounds belong to the class of flavonoids and can be divided into these five groups: flavanones, flavones, flavonols, flavanols, isoflavones and anthocyanidins. Extracts from citrus fruits are usually used as functional ingredients for several products. The aim of this paper was to develop an UHPLC-UV-ESI-HRMS method to define the metabolite profile of different parts of citrus fruit, of a particular cultivar called 'Ovale Calabrese', and in its main by-products. The high resolution mass spectrometry analysis allowed the identification of 27 compounds belonging to the classes of flavonoids and terpenoids. The high contents of phytochemical compounds, reveal the potential use of the 'Ovale Calabrese' as a rich source of nutraceutical compounds.

Research paper thumbnail of Selective extraction of high-value phenolic compounds from distillation wastewater of basil (Ocimum basilicum L.) by pressurized liquid extraction

Electrophoresis, Jan 31, 2018

During the essential oil steam distillation from aromatic herbs, huge amounts of distillation was... more During the essential oil steam distillation from aromatic herbs, huge amounts of distillation wastewaters (DWWs) are generated. These by-products represent an exceptionally rich source of phenolic compounds such as rosmarinic acid (RA) and caffeic acid (CA). Herein, the alternative use of dried basil DWWs (dDWWs) to perform a selective extraction of RA and CA by pressurized liquid extraction (PLE) employing bio-based solvent was studied. To select the most suitable solvent for PLE, the theoretical modelling of Hansen solubility parameters (HSP) was carried out. This approach allows reducing the list of candidate to two solvents: ethanol and ethyl lactate. Due to the composition of the sample, mixtures of water with those solvents were also tested. An enriched PLE extract in RA (23.90 ± 2.06 mg/g extract) with an extraction efficiency of 75.89 ± 16.03% employing a water-ethanol mixture 25:75 (% v/v) at 50°C was obtained. In the case of CA, a PLE extract with 2.42 ± 0.04 mg/g extract,...

Research paper thumbnail of Occurrence of aflatoxin M1 in milk samples from Italy analysed by online-SPE UHPLC-MS/MS

Natural product research, Jan 17, 2017

The occurrence of aflatoxin M1 in 69 milk samples collected in a south region of Italy in 2016 wa... more The occurrence of aflatoxin M1 in 69 milk samples collected in a south region of Italy in 2016 was evaluated. The samples were analysed using an automated method based on online SPE coupled with UHPLC tandem mass spectrometry. After a salt induced liquid-liquid extraction with acetonitrile to remove protein from milk, the extract was diluted with water and analysed using an automated online SPE MS/MS method. Among the analysed samples no one had AFM1 higher than the legally allowable limits whereas 71.4% of the other analysed samples were above the LOD of the method. The highest contamination level of AFM1 was found in pasteurised milk (44.39 ng kg-1). The results show the worrying and widespread of AFM1 contamination, highlighting the necessity of monitoring studies in order to evaluate the reduction of the maximum legal limit.

Research paper thumbnail of Rapid and automated on-line solid phase extraction HPLC-MS/MS with peak focusing for the determination of ochratoxin A in wine samples

Food chemistry, 2018

This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS m... more This study reports a fast and automated analytical procedure based on an on-line SPE-HPLC-MS/MS method for the automatic pre-concentration, clean up and sensitive determination of OTA in wine. The amount of OTA contained in 100μL of sample (pH≅5.5) was retained and concentrated on an Oasis MAX SPE cartridge. After a washing step to remove matrix interferents, the analyte was eluted in back-flush mode and the eluent from the SPE column was diluted through a mixing Tee, using an aqueous solution before the chromatographic separation achieved on a monolithic column. The developed method has been validated according to EU regulation N. 519/2014 and applied for the analysis of 41 red and 17 white wines. The developed method features minimal sample handling, low solvent consumption, high sample throughput, low analysis cost and provides an accurate and highly selective results.

Research paper thumbnail of Focusing and non-focusing modulation strategies for the improvement of on-line two-dimensional hydrophilic interaction chromatography × reversed phase profiling of complex food samples

Analytica chimica acta, Jan 8, 2017

Comprehensive two-dimensional liquid chromatography (LC × LC) is ever gaining interest in food an... more Comprehensive two-dimensional liquid chromatography (LC × LC) is ever gaining interest in food analysis, as often, food-related samples are too complex to be analyzed through one-dimensional approaches. The use of hydrophilic interaction chromatography (HILIC) combined with reversed phase (RP) separations has already been demonstrated as a very orthogonal combination, which allows attaining increased resolving power. However, this coupling encompasses different analytical challenges, mainly related to the important solvent strength mismatch between the two dimensions, besides those common to every LC × LC method. In the present contribution, different strategies are proposed and compared to further increase HILIC × RP method performance for the analysis of complex food samples, using licorice as a model sample. The influence of different parameters in non-focusing modulation methods based on sampling loops, as well as under focusing modulation, through the use of trapping columns in...

Research paper thumbnail of Oil distillation wastewaters from aromatic herbs as new natural source of antioxidant compounds

Food research international (Ottawa, Ont.), 2017

Distillation wastewaters (DWWs) are generated during the essential oil steam distillation from ar... more Distillation wastewaters (DWWs) are generated during the essential oil steam distillation from aromatic herbs. Despite of growing interest on novel source of natural antioxidant compounds as food additives, studies on DWWs are scarse. Herein, the potential of DWWs produced by the distillation of packaged fresh basil, rosemary and sage wastes was evaluated by chemical and antioxidant characterization. HPLC-DAD-HRMS profiling revealed that DWWs contain water-soluble phenolic compounds, mainly caffeic acid derivatives and flavonoid glycosides, with rosmarinic acid (RA) as predominant components (29-135mg/100mL). DWWs demonstrated high levels of total phenolic compounds (TPC, 152-443mg GAE/100mL) and strong antioxidant capacities, in ORAC, DPPH and ABTS assays (1101-4720, 635-4244 and 571-3145μmol TE/100mL, respectively). Highly significant correlations of TEAC values with TPC and RA contents revealed that phenolic compounds and high RA content were responsible of DWWs antioxidant prope...

Research paper thumbnail of Metabolite profiling of licorice (Glycyrrhiza glabra) from different locations using comprehensive two-dimensional liquid chromatography coupled to diode array and tandem mass spectrometry detection

Analytica Chimica Acta, 2016

profiling of licorice (Glycyrrhiza glabra) from different locations using comprehensive two-dimen... more profiling of licorice (Glycyrrhiza glabra) from different locations using comprehensive two-dimensional liquid chromatography coupled to diode array and tandem mass spectrometry detection,

Research paper thumbnail of A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography–tandem mass spectrometry

Analytical and Bioanalytical Chemistry, 2015

According to current demands and future perspectives in food safety, this study reports a fast an... more According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30 %) at 110°C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103 %) and repeatability (RSD<8, n=3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling highthroughput analysis and highly accurate and precise results.

Research paper thumbnail of Fragmentation pathways of polycyclic polyisoprenylated benzophenones and degradation profile of nemorosone by multiple-stage tandem mass spectrometry

Journal of the American Society for Mass Spectrometry, 2009

Research paper thumbnail of New Lignans from the Roots of Valeriana prionophylla with Antioxidative and Vasorelaxant Activities

Journal of Natural Products, 2004

Two new 7,9&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;a... more Two new 7,9&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;:7&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;,9-diepoxylignan glycosides have been isolated from the roots of Valeriana prionophylla. Their structures have been established on the basis of 1D and 2D NMR experiments as prinsepiol-4-O-beta-D-glucopyranoside (1) and fraxiresinol-4&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;-O-beta-D-glucopyranoside (2). In addition, 8-hydroxypinoresinol-4&amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;#39;-O-beta-d-glucopyranoside (3), 8-hydroxypinoresinol (4), prinsepiol (5), and chlorogenic acid were isolated. Compounds 1, 3, 4, and 5 were evaluated for their antioxidative properties in Trolox equivalent antioxidant activity (TEAC) and chemiluminescence (CL) assays. The same compounds were tested for their vascular activity in rat aorta rings. The aglycones 4 and 5 displayed powerful antioxidant activity; in addition, aglycone 4 showed a higher vasorelaxant activity than compounds 1, 3, and 5.