Investigating the in vitro bioaccessibility of polyphenols in fresh and sun‐dried figs (Ficus carica L.)

In this study, in order to evaluate the in vitro bioaccessibility of fresh and sun‐dried figs, total antioxidant capacity (TAC), total proanthocyanidin content (TPA) and the major phenolic compounds were determined at different phases of simulated gastrointestinal (GI) tract digestion for Sarilop and Bursa siyahi fig varieties. Four major phenolic compounds (chlorogenic acid, rutin, cyanidin‐3‐glucoside (C3G) and cyanidin‐3‐rutinoside (C3R)) were investigated for GI tract digestion. The results of in vitro GI tract digestion revealed that the dialysed fraction (IN) represented 9–26% and 1–22% of the initial TAC of the whole‐fresh yellow and purple figs, respectively. Moreover, in case of 2,2‐azinobis(3‐ethylbenzothiazoline)‐6‐sulphonic acid (ABTS), TPA and chlorogenic acid contents, drying caused an increase in the IN fraction of yellow figs (38, 140, 50%, respectively). The bioaccessibility of C3G and C3R were quite low for fresh figs (0–5% of the initial values), whereas for dried figs, anthocyanins were not detected at all in the IN fraction.     

Changes in pigment profile and surface colour of fig (Ficus carica L.) during drying

In this study, anthocyanins in three fresh fig varieties (Ficus carica L.) cultivated in Turkey were characterised and quantified by HPLC/DAD and HPLC/MS. In addition, the carotenoid composition of Sar?lop and Sar?zeybek, yellow fig varieties, was determined, and then the ripening‐ and drying‐related changes in carotenoids and surface colour of figs were monitored during conventional sun‐drying. Four different anthocyanins, cyanidin‐3‐glucoside, cyanidin‐3,5‐diglucoside, cyanidin‐3‐rutinoside (major anthocyanin) and pelargonidin‐3‐glucoside, were identified in samples. Lutein, zeaxanthin, β‐cryptoxanthin and β‐carotene were carotenoids in yellow fig varieties. Approximately 80% of carotenoid compounds in yellow fig varieties degraded at the end of drying (i.e. seventh day). L (lightness), a (redness and greenness) and b (yellowness and blueness) colour parameters were measured by Hunter Lab system. Great changes in carotenoid composition and surface colour were observed at ripening stage on tree. A significant reduction in L and b values that refers to browning in figs was made in the first 3 days of drying process.     

Sensory Profiles for Dried Fig (Ficus carica L.) Cultivars Commercially Grown and Processed in California

A trained sensory panel evaluated the 6 fig cultivars currently sold in the California dried fig market. The main flavor and aroma attributes determined by the sensory panel were “caramel,” “honey,” “raisin,” and “fig,” with additional aroma attributes: “common date,” “dried plum,” and “molasses.” Sensory differences were observed between dried fig cultivars. All figs were processed by 2 commercial handlers. Processing included potassium sorbate as a preservative and SO₂ application as an antibrowning agent for white cultivars. As a consequence of SO₂ use during processing, high sulfite residues affected the sensory profiles of the white dried fig cultivars. Significant differences between dried fig cultivars and sources demonstrate perceived differences between processing and storage methods. The panel‐determined sensory lexicon can help with California fig marketing.     

Characterisation of phenolic extracts from olive pulp and olive pomace by electrospray mass spectrometry

Methanol extracts of olive pomace (two‐phase olive oil extraction) and olive pulp were analysed by reverse phase HPLC and the eluted fractions were characterised by electrospray ionisation mass spectrometry. This technique allowed the identification of some common phenolic compounds, namely, verbascoside, rutin, caffeoyl‐quinic acid, luteolin‐4‐glucoside and 11‐methyl‐oleoside. Hydroxytyrosol‐1′‐β‐glucoside, luteolin‐7‐rutinoside and oleoside were also detected. Moreover, this technique enabled the identification, for the first time in Olea europaea tissues, of two oleoside derivatives, 6′‐β‐glucopyranosyl‐oleoside and 6′‐β‐rhamnopyranosyl‐oleoside, and of 10‐hydroxy‐oleuropein. Also, an oleuropein glucoside that had previously been identified in olive leaves was now detected in olive fruit, both in olive pulp and olive pomace. With the exception of oleoside and oleuropein, the majority of phenolic compounds were found to occur in equivalent amounts in olive pulp and olive pomace. Oleoside was the main phenolic compound in olive pulp (31.6 mg g^?1) but was reduced to 3.6 mg g^?1 in olive pomace, and oleuropein (2.7 mg g^?1 in the pulp) almost disappeared (<0.1 mg g^?1 in the pomace). Both these phenolic compounds were degraded during the olive oil extraction process. Copyright © 2004 Society of Chemical Industry     

Quality attributes and their relations in fresh black ripe ‘Kalamon’ olives (Olea europaea L.) for table use – phenolic compounds and total antioxidant capacity

Quality attributes were investigated in fresh Greek black table ‘Kalamon’ olives prior to processing. Fruit weight, dimensions, respiration and ethylene production rates, firmness, peel colour, moisture, oil content, total antioxidant capacity (TAC), the concentration of total phenolics (TP) and phenolic compounds (hydroxytyrosol, oleuropein, tyrosol, verbascoside, luteolin‐7‐O‐glucoside, luteolin, rutin) were determined in olives from different orchards. There was a significant effect of orchard on most attributes, but not on fruit firmness. Verbascoside, oleuropein and hydroxytyrosol were the major phenolics, and the presence of verbascoside in ‘Kalamon’ olives is revealed for the first time. Positive correlations were found among fruit weight, dimensions, respiration and ethylene. TAC was positively related mainly to TP, hydroxytyrosol, verbascoside and rutin, but inversely to oleuropein. Luteolin was inversely related to luteolin‐7‐O‐glucoside. Colour darkening was directly related to TAC, while colour parameters were positively and moderately affected by oil and moisture.     

Phenolic compound content of fresh and dried figs (Ficus carica L.)

Eighteen fig cultivars commonly grown in the south-eastern Spain were collected in two crops (spring and summer) and their polyphenolic profile was determined. Fruit from the first crop generally showed higher phenolic values than those from the second. Higher concentrations of total phenolics were found in skin than in flesh. LC–UV-DAD/ESI-MSⁿ analysis of the figs pointed to a high anthocyanin content, mainly cyanidin-3-rutinoside, flavonols such as quercetin-rutinoside, phenolic acids such as chlorogenic acid and flavones like luteolin 6C-hexose-8C-pentose and apigenin-rutinoside. The c-glycosides have not been previously described in figs. Moreover, to compare intact proanthocyanidins and proanthocyanin cleavage products, an acid-catalysis was made in the presence of phloroglucinol (phloroglucinolysis) and the mean degree of polymerisation was calculated. Finally, three cultivars of dried figs were also studied.     

Carry-Over of Aflatoxins to Fig Molasses from Contaminated Dried Figs

The carry-over of aflatoxins to fig molasses produced by using two different processing techniques from contaminated dried figs (> 1000 ppb of total aflatoxins) were examined by using a HPLC technique. The effects of extraction, bleaching and concentration steps on the reduction of aflatoxin levels were also investigated. The reductions in total aflatoxin levels in fig molasses produced by using the two techniques were detected to be 62 and 38%, respectively. Extraction, bleaching and concentration steps were observed to cause 22% reduction in total aflatoxin levels.     

Authentication of Geographical Origin and Crop System of Grape Juices by Phenolic Compounds and Antioxidant Activity Using Chemometrics

The main goal of this work was to propose an authentication model based on the phenolic composition and antioxidant and metal chelating capacities of purple grape juices produced in Brazil and Europe in order to assess their typicality. For this purpose, organic, conventional, and biodynamic grape juices produced in Brazil (n = 65) and in Europe (n = 31) were analyzed and different multivariate class‐modeling and classification statistical techniques were employed to differentiate juices based on the geographical origin and crop system. Overall, Brazilian juices, regardless of the crop system adopted, presented higher contents of total phenolic compounds and flavonoids, total monomeric anthocyanins, proanthocyanidins, flavonols, flavanols, cyanidin‐3‐glucoside, delphinidin‐3‐glucoside, and malvidin‐3,5‐glucoside. No differences were observed for trans‐resveratrol, malvidin‐3‐glucoside, and pelargonidin‐3‐glucoside between countries and among crop systems. A total of 91% of Brazilian and 97% of European juices were adroitly classified using partial least squares discriminant analysis when the producing region was considered (92% efficiency), in which the free‐radical scavenging activity toward 2,2‐diphenyl‐1‐picrylhydrazyl, content of total phenolic compounds, gallic acid, and malvidin‐3‐glucoside were the variables responsible for the classification. Intraregional models based on soft independent modeling of class analogy were able to differentiate organic from conventional Brazilian juices as well as conventional and organic/biodynamic European juices.     

The analysis of phenolic compounds in daylily using UHPLC‐HRMSn and evaluation of drying processing method by fingerprinting and metabolomic approaches

The flowers of daylily (Hemerocallis fulva (L.) L.) are called “Jinzhen” which are commonly used as vegetables or seasoning in East Asia. In this study, we evaluated the chemical profile changes with different processing method after harvest. Five different drying methods including solar drying, vacuum freeze drying, steam drying, and hot air drying method were investigated regarding their impact on the chemical constituents in daylily. The major phenolic compounds were tentatively characterized with ultra‐high performance liquid chromatography tandem high‐resolution mass spectrometric with multistage fragmentation techniques (UHPLC‐HRMSⁿ). The UHPLC‐UV fingerprinting and UHPLC‐HRMSⁿ‐based metabolomic approaches were used for identifying the difference between different processing methods. The quercetin 3‐O‐rutinoside, 5‐O‐caffeoylquinic acids are obviously higher in freeze‐dried and steam‐dried samples. Colchicine was believed to be one of the toxic constituents found in daylily fresh flowers; however, no colchicine was found in any the daylily samples investigated.

Practical applications

The drying process is particularly important for handling and distribution of daylily flowers after harvest and it can also prolong the shelf life. However, the drying process may result in degradation of nutrients and quality loss in food. Steamed sunlight dried or hot air drying methods preserve most of the phenolic composition of fresh daylily samples. The purpose of this study was to analyze the phenolic compounds in daylily using ultra‐high performance liquid chromatography tandem high‐resolution mass spectrometric with multistage fragmentation techniques and to evaluate the drying processing method by fingerprinting and metabolomic approaches.     

Nutritional Compounds in Figs from the Southern Mediterranean Region

Nutritive value of mature figs (Ficus carica L.) was investigated in five Tunisian cultivars, ‘Bouhouli’ (BHL) and ‘Zidi’ (ZD) (dark skin figs); ‘Thgagli’ (THG), ‘Bidhi’ (BD), and ‘Khedri’ (KHD) (yellow-green skin figs). Sugars, organic acids, fibres, and polyphenols were analysed in representative fruit samples from two distinct regions known to develop fig crops. Tunisian figs were characterized by predominance of glucose (6.30 g/100 g fresh weight) and fructose (5.10 g/100 g fresh weight). Citric acid (0.35 g/100 g fresh weight) was the major organic acid in all cultivars, almost three times higher than malic acid (0.13 g/100 g fresh weight). Average content of alcohol insoluble solids was 3.3 g/100 g FW. Four main polyphenols could be identified: two anthocyanins (cyanidin-3-glucoside; cyanidin-3-rutinoside), one flavonol (rutin), and one hydroxycinnamic acid (5-cafeoylquinic acid), revealed only in ‘BD’ samples. Cyanidin-3-rutinoside was the most abundant compound among all cultivars. Compared to common fruit, figs are among high sugar leveled fruit with significant dietary fibre content. Dark skin ‘ZD’ fruit were the most interesting figs with the highest concentration of sugars, organic acids, and polyphenols, especially cyanidin-3-rutinoside. This cultivar could be better advised for fresh consumption. However, the three lighter cultivars are more suitable for drying.     

Wild Prunus Fruit Species as a Rich Source of Bioactive Compounds

Sugars, organic acids, carotenoids, tocopherols, chlorophylls, and phenolic compounds were quantified in fruit of 4 wild growing Prunus species (wild cherry, bird cherry, blackthorn, and mahaleb cherry) using HPLC‐DAD‐MSn. In wild Prunus, the major sugars were glucose and fructose, whereas malic and citric acids dominated among organic acids. The most abundant classes of phenolic compounds in the analyzed fruit species were anthocyanins, flavonols, derivatives of cinnamic acids, and flavanols. Two major groups of anthocyanins measured in Prunus fruits were cyanidin‐3‐rutinoside and cyanidin‐3‐glucoside. Flavonols were represented by 19 derivatives of quercetin, 10 derivatives of kaempferol, and 2 derivatives of isorhamnetin. The highest total flavonol content was measured in mahaleb cherry and bird cherry, followed by blackthorn and wild cherry fruit. Total phenolic content varied from 2373 (wild cherry) to 11053 mg GAE per kg (bird cherry) and ferric reducing antioxidant power antioxidant activity from 7.26 to 31.54 mM trolox equivalents per kg fruits.     

Determination of antioxidant activity and phenolic compounds of Muntingia calabura Linn. peel by HPLC‐DAD and UPLC‐ESI‐MS/MS

Antioxidant activity in Muntingia calabura Linn. peel was evaluated by DPPH radical, ORAC, ABTS cation radical, FRAP assays and total phenolic contents by different extraction conditions. In addition, a method for determination of phenolic compounds in calabura peel samples harvested in Brazil using methanol:water and magnetic stirring as the extraction method, HPLC‐DAD and UPLC‐ESI‐MS/MS analysis were developed. Calabura peel showed antioxidant activity for all extraction conditions and assays evaluated, the most polar solvents being more effective. The developed HPLC‐DAD method allowed the accurate determination of phenolic compounds, with recoveries in the range of 72–107% and precision values ≤4%, with exception for chlorogenic acid. Gallic acid was determined at the highest concentration levels, followed by myricetin, ferulic acid and vanillic acid. However, all the five proposed phenolic compounds were identified in calabura peel samples by UPLC‐ESI‐MS/MS. Thus, calabura peel, an uncommon edible fruit part, can be appointed as a rich source of phenolic compounds.     

Changes in aromatic profile of fresh and dried fig – the role of pre‐treatments in drying process

The aromatic profile of volatiles in fresh figs (FF), fresh figs frozen in liquid nitrogen (NF) and dried figs (DF) (dark variety Petrova?a Crna) was characterised by HS–SPME followed by GC–MS. Figs were dried in a pilot plant cabinet dryer using different pre‐treatments to preserve the dried fruit: sulphuring and immersion in a solution of citric acid and ascorbic acid (separately). The adaptability of thin‐layer drying models to whole figs was investigated. Fresh figs and fresh figs frozen in liquid nitrogen differed mainly in the amount of aldehydes. The highest abundance of volatile compounds in dried figs was found in figs pre‐treated with sulphur dioxide and the control, compared to samples immersed in the acid solutions. Preservation was the most successful for the group of terpenes and terpenic compounds, quite good for some esters and ketones, whereas aldehydes were not affected by the used pre‐treatment.     

Phenolic Compounds,Volatiles, and Sensory Characteristics of Twelve Sweet Cherry (Prunus avium L.) Cultivars Grown in Turkey

The paper reports the phenolic, anthocyanin, and volatile compounds and sensory characteristics of 12 cultivars of sweet cherries including cvs. Belge, Bing, Dalbasti, Durona di Cesena, Lambert, Merton Late, Starks Gold, Summit, Sweetheart, Van, Vista, and 0–900 Ziraat. Eight individual phenolic compounds were determined by the HPLC‐DAD method. Among these cherries, cvs. Bing, Durona di Cesena, and Lambert contained higher levels of total individual phenolic compounds than the other cultivars. Six anthocyanins were detected in cherries and cyanidin‐3‐O‐rutinoside was principal and it was the highest level in cv. Bing. The major volatiles found were 1‐hexanol, (E)‐2‐hexen‐1‐ol, benzylalcohol, hexenal, (E)‐2‐hexenal, and benzaldehyde. Sensory evaluation of the cherries showed that cvs. Belge, Bing, Dalbasti, and Summit have higher textural and flavor scores than others. It was concluded that the same compounds for phenolic or volatiles profiles of sweet cherries were similar in qualitative; however, quantitative differences were observed in these cultivars.     

Enrichment of fresh pasta with antioxidant extracts obtained from artichoke canning by‐products by ultrasound‐assisted technology and quality characterisation of the end product

This work is aimed at: (i) analysing the extracts obtained from canning by‐products of three artichoke cultivars (Opal, Capriccio and Catanese) for antioxidant parameters; (ii) comparing UHPLC‐ESI‐MS/MS profile, colour, textural properties and cooking performance of fresh pasta enriched of the most antioxidant extract, with control pasta. The concentrated Catanese cv. extracts showed the highest antioxidant activity (1662 μmol Trolox equivalents L^?1) and the highest levels of luteolin‐7‐O‐rutinoside, luteolin‐7‐O‐glucoside and apigenin‐7‐O‐rutinoside compared to other cultivars. Fresh pasta enriched of Catanese extract showed higher (P < 0.05) phenolic compounds and antioxidant activity (500 mg gallic acid kg^?1 and 1324 μmol Trolox kg^?1, respectively) than control pasta (306 mg gallic acid kg^?1 and 886 μmol Trolox kg^?1, respectively). The extract increased (P < 0.05) pasta brownness (from 19.93 to 23.34), and decreased yellowness (from 27.11 to 23.09), but did not alter textural and cooking parameters. So, pasta was a good vehicle to increase the antioxidant dietary intake.     

Changes in Radical-scavenging Activity and Components of Mulberry Fruit During Maturation

ABSTRACT Extracts of mulberry fruits (Morus sp.) were prepared from 8 cultivars harvested at 4 stages of maturity, and their radicalscavenging activity, anthocyanin content, and total phenolic content were measured. The radical‐scavenging activity was evaluated by a spectrophotometric assay using the 1,1‐diphenyl‐2‐picrylhydrazyl radical (DPPH) in a 96‐well microplate. Mulberry fruit extracts exhibited the DPPH‐scavenging activities, ranging from 2.5 to 20.3 μmol‐Trolox equiv/g‐FW. Their activities were variable during maturation, and the highest activity was observed in the fully mature mulberry fruit in all cultivars. Anthocyanin was scarcely present in the immature mulberry fruits; however, its content increased as the fruit matured in all cultivars. On the other hand, all immature mulberry fruits contained non‐anthocyanin phenolic compound. An on‐line high‐performance liquid chromatography (HPLC) method for the detection of DPPH‐scavenging compounds revealed the difference in predominant radical scavengers between the immature and fully mature stages in the Miran 5 cultivar. Four major radical scavengers in the Miran 5 cultivar were assigned to 2 caffeoylquinic acids (chlorogenic acid and its isomer) and 2 anthocyanins (cyanidin 3‐glucoside and cyanidin 3‐rutinoside) in the immature and fully mature stages, respectively, by LC‐ESI‐MS/MS analysis. The change in the content of 4 compounds in mulberry fruits during maturation demonstrated that the most likely contributors to the DPPH‐scavenging activity were caffeoylquinic acids in the immature mulberry and anthocyanins in the mature and fully mature mulberry.     

Syringa oblata Lindl var. alba as a source of oleuropein and related compounds

The leaf methanol extract of Syringa oblata Lindl var. alba was investigated as a source of oleuropein and related compounds. The extract had a high total phenol content and a radical scavenging activity similar to that of the respective extract from Olea europaea leaves. HPLC‐DAD characterisation of the two most abundant phenolic compounds in the extract of S. oblata indicated that both had UV spectra matching that of oleuropein. The presence of oleuropein was verified by using LC‐MS. Identification of the second compound was only feasible after isolation (preparative HPLC) and spectroscopic characterisation [LC‐MS, ¹H NMR and homonuclear two‐dimensional correlated spectroscopy (COSY)]. The compound identified was the known bioactive syringopicroside. On the basis of MS data other peaks were assigned to oleuropein aglycone, verbascoside, ligstroside and syringopicroside derivatives, as well as to a luteolin rutinoside. The findings are promising for the potential exploitation of S. oblata leaf extract as a source for oleuropein and other bioactive ingredients. Copyright © 2006 Society of Chemical Industry     

Polyphenol composition of peel and pulp of two Italian fresh fig fruits cultivars (<Emphasis Type="Italic">Ficus carica</Emphasis> L.)

An analytical study was carried out on phenols in two fig cultivars (Ficus carica L.), one black and one green. Fresh fruits were peeled and phenols were extracted separately from the peel and the pulp. The extracts were subjected to HPLC-DAD analysis, by monitoring at four wavelengths, 280, 316, 365 and 520 nm for catechins and benzoic acids, hydroxycinnamic acids, flavonols and anthocyanins, respectively. Results showed that phenols are concentrated almost exclusively in the peel, with the black cultivar having the highest content. In particular, the peel was rich in rutin, with amounts from 527 to 1,071 mg/kg (fresh basis) for green and black figs, respectively. The peel of black figs showed an appreciable content of cyanidin 3-O-rutinoside. The pulp of both green and black cultivars contained only cyanidin 3-O-rutinoside, while the cyanidin 3-O-glucoside was found only in the peel of the black figs. Chlorogenic acid and another cinnamic acid were detected in the peel of both cultivars, while benzoic acids and catechins were not present. Alessandra Del Caro and Antonio Piga contributed equally to this study.     

Development of a green two‐dimensional HPLC‐DAD/ESI‐MS method for the determination of anthocyanins from Prunus cerasifera var. atropurpurea leaf and improvement of their stability in energy drinks

This study aimed to develop a green two‐dimensional HPLC‐DAD/ESI‐MS method for analysing anthocyanins from Prunus cerasifera var. atropurpurea leaf and improve their stability in energy drinks by the addition of phenolic acids. Ethanol and tartaric acid solutions were used as mobile phases for one‐dimensional HPLC‐DAD for quantitative analysis of anthocyanins, and the primary anthocyanins were identified as cyanidin‐3‐O‐galactoside, cyanidin‐3‐O‐glucoside and cyanidin‐3‐O‐rutinoside using two‐dimensional HPLC‐MS. Method validation showed that the developed method was accurate, stable and reliable for the analysis of P. cerasifera anthocyanins. The effects of gallic, ferulic and caffeic acid on the stability of cyanidin‐3‐O‐galactoside, cyanidin‐3‐O‐glucoside, cyanidin‐3‐O‐rutinoside and total anthocyanins from P. cerasifera leaf in energy drinks were evaluated, and the degradation of P. cerasifera anthocyanins ideally followed a first‐order model (R² > 0.98). Gallic acid showed stronger protective effects on P. cerasifera anthocyanins in energy drinks, and adding/increasing ferulic and caffeic acids accelerated the degradation reactions.