UPLC-MS2 Profiling of Blackthorn Flower Polyphenols Isolated by Ultrasound-Assisted Extraction.

Ultrasound-assisted extraction (UAE) was optimized for fast and effective isolation of blackthorn flower polyphenols. The effects of ethanol concentration (50% and 70%) in extraction solvent, ultrasound amplitude (50%, 75%, and 100%) and extraction time (3, 6, and 9 min) were evaluated. UPLC-MS2 was used to determine phenolic profile of blackthorn flowers extracts. A total of 28 different phenolic compounds were identified, belonging to the classes of hydroxycinnamic acids, flavonol glycosides and flavanols. Kaempferol and quercetin derivatives were the most abundant compounds represented by kaempferol-pentoside and rhamnoside in concentrations up to 494.94 and 436.62 mg/100 g and quercetin-pentoside in concentration up to 226.75 mg/100 g. Observed parameters of UAE did not affect the qualitative phenolic composition of blackthorn flower extracts. On the contrary, the concentration of polyphenols increased with higher ethanol concentration in solvent, higher ultrasound amplitude and prolongation of extraction time. The established conditions for optimal extraction of blackthorn flower polyphenols using ultrasound were: 70% ethanol as extraction solvent, 75% of ultrasound amplitude and 9 min extraction time, resulting in extract rich in polyphenols with a great potential for use in pharmaceutical and food industry. PRACTICAL APPLICATION: In this study, ultrasound-assisted extraction (UAE) was optimized in order to establish fast and effective method for production of crude blackthorn flower extract rich in polyphenols. UPLC-MS2 analysis showed 28 different phenolic compounds belonging to the classes of hydroxycinnamic acids, flavonol glycosides, and flavanols with quercetin and kaempferol glycosides in the highest concentrations, implicating high potential of blackthorn flowers' extract for use in food and pharmaceutical industries.

[1]  V. Dragović-Uzelac,et al.  Retention of polyphenols in encapsulated sour cherry juice in dependence of drying temperature and wall material , 2017 .

[2]  D. Kovačević,et al.  Effect of Microwave-Assisted Extraction on the Phenolic Compounds and Antioxidant Capacity of Blackthorn Flowers. , 2017, Food technology and biotechnology.

[3]  M. Ferreiro-González,et al.  Optimization of the ultrasound-assisted extraction of anthocyanins and total phenolic compounds in mulberry (Morus nigra) pulp. , 2017, Food chemistry.

[4]  Hua-Bin Li,et al.  Ultrasound-assisted extraction of natural antioxidants from the flower of Limonium sinuatum: Optimization and comparison with conventional methods. , 2017, Food chemistry.

[5]  F. Barba,et al.  HPLC-DAD-ESI-MS(2) analytical profile of extracts obtained from purple sweet potato after green ultrasound-assisted extraction. , 2017, Food chemistry.

[6]  F. Barba,et al.  Recovery of colorants from red prickly pear peels and pulps enhanced by pulsed electric field and ultrasound , 2016 .

[7]  Jin Liang,et al.  Optimization of Ultrasound-Assisted Extraction of phenolic compounds and anthocyanins from blueberry (Vaccinium ashei) wine pomace. , 2016, Food chemistry.

[8]  M. T. Machado,et al.  Ultrasound assisted extraction and nanofiltration of phenolic compounds from artichoke solid wastes , 2016 .

[9]  A. Oniszczuk,et al.  Optimization of ultrasound-assisted extraction and LC-ESI–MS/MS analysis of phenolic acids from Brassica oleracea L. var. sabellica , 2016 .

[10]  Francisco J. Barba,et al.  Green alternative methods for the extraction of antioxidant bioactive compounds from winery wastes and by-products: A review , 2016 .

[11]  B. Pavlić,et al.  Optimization of ultrasound-assisted extraction of bioactive compounds from wild garlic (Allium ursinum L.). , 2016, Ultrasonics sonochemistry.

[12]  Brijesh K. Tiwari,et al.  Clean recovery of antioxidant compounds from plant foods, by-products and algae assisted by ultrasounds processing. Modeling approaches to optimize processing conditions , 2015 .

[13]  M. Brnčić,et al.  Optimization of Ultrasound Assisted Extraction of Functional Ingredients from Stevia Rebaudiana Bertoni Leaves , 2015 .

[14]  F. Barba,et al.  Effect of Alternative Physical Treatments (Ultrasounds, Pulsed Electric Fields, and High-Voltage Electrical Discharges) on Selective Recovery of Bio-compounds from Fermented Grape Pomace , 2015, Food and Bioprocess Technology.

[15]  V. Rathod,et al.  Ultrasound assisted production of a fibrinolytic enzyme in a bioreactor. , 2015, Ultrasonics sonochemistry.

[16]  S. Mitić,et al.  Phenolic composition, antioxidant and antimicrobial activity of the extracts from Prunus spinosa L. fruit , 2014 .

[17]  E. Sikora,et al.  Composition and antioxidant properties of fresh and frozen stored blackthorn fruits (Prunus spinosa L.) , 2013 .

[18]  A. Jambrak,et al.  The effect of microwave assisted extraction on the isolation of anthocyanins and phenolic acids from sour cherry Marasca (Prunus cerasus var. Marasca) , 2013 .

[19]  S. Karlović,et al.  Ultrasound-Assisted Infrared Drying of Pear Slices: Textural Issues , 2013 .

[20]  Qinan Wu,et al.  Optimisation of ultrasound assisted extraction of phenolic compounds from Sparganii rhizoma with response surface methodology. , 2013, Ultrasonics sonochemistry.

[21]  Marijana Jukić,et al.  The Influence of Microwave-Assisted Extraction on the Isolation of Sage (Salvia officinalis L.) Polyphenols , 2012 .

[22]  M. Palma,et al.  Ultrasound assisted extraction of phenolic compounds from grapes. , 2012, Analytica chimica acta.

[23]  Ana Maria Carvalho,et al.  Characterization of phenolic compounds in flowers of wild medicinal plants from Northeastern Portugal. , 2012, Food and chemical toxicology : an international journal published for the British Industrial Biological Research Association.

[24]  Catherine Barry-Ryan,et al.  Optimization of ultrasound assisted extraction of antioxidant compounds from marjoram (Origanum majorana L.) using response surface methodology. , 2012, Ultrasonics sonochemistry.

[25]  G. Justino,et al.  Structural Analysis of Flavonoids and Related Compounds - A Review of Spectroscopic Applications , 2012 .

[26]  A. Ismail,et al.  Response surface optimisation for the extraction of phenolic compounds and antioxidant capacities of underutilised Mangifera pajang Kosterm. peels. , 2011 .

[27]  Farid Chemat,et al.  Applications of ultrasound in food technology: Processing, preservation and extraction. , 2011, Ultrasonics sonochemistry.

[28]  C. Piñol,et al.  Rapid methods to determine procyanidins, anthocyanins, theobromine and caffeine in rat tissues by liquid chromatography-tandem mass spectrometry. , 2011, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[29]  F. Priego-Capote,et al.  The role of ultrasound in analytical derivatizations. , 2011, Journal of chromatography. B, Analytical technologies in the biomedical and life sciences.

[30]  M. Biesaga Influence of extraction methods on stability of flavonoids. , 2011, Journal of chromatography. A.

[31]  Anet Režek Jambrak,et al.  Experimental Design and Optimization of Ultrasound Treatment of Food Products , 2011 .

[32]  G. Schmeda-Hirschmann,et al.  Direct identification of phenolic constituents in Boldo Folium (Peumus boldus Mol.) infusions by high-performance liquid chromatography with diode array detection and electrospray ionization tandem mass spectrometry. , 2010, Journal of chromatography. A.

[33]  G. Majetich,et al.  Optimization of ultrasonic-assisted extraction of chlorogenic acid from Folium eucommiae and evaluation of its antioxidant activity , 2010 .

[34]  J. Jahim,et al.  Extraction of hydrolysable tannins from Phyllanthus niruri Linn.: Effects of solvents and extraction methods , 2007 .

[35]  Ferran Sánchez-Rabaneda,et al.  Separation and characterization of phenolic compounds in fennel (Foeniculum vulgare) using liquid chromatography-negative electrospray ionization tandem mass spectrometry. , 2004, Journal of agricultural and food chemistry.

[36]  M. Clifford,et al.  Hierarchical scheme for LC-MSn identification of chlorogenic acids. , 2003, Journal of agricultural and food chemistry.

[37]  M. Olszewska,et al.  Flavonoids from the flowers of Prunus spinosa L. , 2001, Acta poloniae pharmaceutica.

[38]  M Vinatoru,et al.  An overview of the ultrasonically assisted extraction of bioactive principles from herbs. , 2001, Ultrasonics sonochemistry.

[39]  T. Mason,et al.  The extraction of rutin from flower buds of Sophora japonica. , 2001, Ultrasonics sonochemistry.

[40]  M. Olszewska,et al.  Quantitative determination of flavonoids in the flowers and leaves of Prunus spinosa L. , 2001, Acta poloniae pharmaceutica.

[41]  D. Ferreira,et al.  A-type proanthocyanidins from Prunus spinosa , 1991 .

[42]  A M Joglekar,et al.  Product excellence through design of experiments , 1987 .