To investigate into the T-2 and HT-2 toxin occurrence, 240 samples of unprocessed cereals (maize, wheat, barley, and oats) were sampled from different fields located in three Croatian regions during ...2017-2018. In all samples, sum concentrations of T-2/HT-2 toxin were determined using the ELISA method, while the LC-MS/MS was used as a confirmatory method for both mycotoxins in positive samples (>LOD) and the establishment of T-2 over HT-2 toxin ratios. The results showed oats to be the most contaminated cereal, with T-2/HT-2 toxins detected in 70.0% of samples, followed by barley (40.9%), maize (26.8%) and wheat (19.2%), with the mean T-2/HT-2 ratio ranging from 1:2.7 in maize to 1:4.4 in oats. Sum T-2/HT-2 concentrations in two maize samples were higher than the indicative level recommended by the European Commission, necessitating subsequent investigations into the conditions under which these poorly investigated mycotoxins are produced. Statistically significantly (
< 0.05) higher concentrations of T-2/HT-2 toxin were determined in oats throughout study regions as compared to those found in wheat, but not maize and barley, while the concentrations of these mycotoxins were related to the regional weather in Croatia.
The endemic brown macroalga
J. Agardh from the Adriatic Sea was in the focus of the present research. The volatiles of fresh (FrFv) and air-dried (DrFv) samples of
obtained by headspace solid-phase ...microextraction (HS-SPME) and hydrodistillation (HD) were analyzed by gas chromatography equipped with flame ionization detector and mass spectrometry (GC-FID/MS). The major HS-FrFv compound was pentadecane (61.90-71.55%) followed by pentadec-1-ene (11.00-7.98%). In HS-DrFv, pentadec-1-ene was not present, and few lower aliphatic compounds appeared, as well as benzaldehyde and benzyl alcohol. In HD-FrFv, particularly abundant were alkenes (such as pentadec-1-ene (19.32%), or (
)-pentadec-7-ene (8.35%)). In HD-DrFv, more oxidation products were present (e.g., carbonyl compounds such as tridecanal (18.51%)). The fatty acids profile of freeze-dried sample (FdFv) after conversion to methyl esters was determined by GC-FID, and oleic acid was dominant (42.28%), followed by arachidonic acid (15.00%). High-performance liquid chromatography-high-resolution mass spectrometry with electrospray ionization (HPLC-ESI-HRMS) was used for the screening of less polar fractions (F3 and F4) of
. Mono- and diglycerides of stearic, palmitic, oleic, and arachidonic acids were found. Terpenoids and steroids comprised the compounds C
H
O
and C
H
O
. Among carotenoids, fucoxanthin was identified. Chlorophyll derivatives were also found (C
H
N
O
), dominated by pheophytin
. The antioxidant activity of the fractions was investigated by in vitro assays (oxygen radical absorbance capacity (ORAC), reduction of radical cation (ABTS•
), 2,2-diphenyl-1-picryl-hydrazyl-hydrate (DPPH) assay, and ferric reducing antioxidant power (FRAP)) and by in vivo zebrafish model (along with fish embryotoxicity). In vitro experiments proved good radical scavenging abilities of F3 and F4 fractions, which were additionally supported by the protective effect against hydrogen peroxide-induced oxidative stress in zebrafish embryos.
In this study, an efficient utilization and valorization of mandarin peel (Citrus unshiu Marc. var. Kuno) was investigated using innovative and green extraction techniques. The first step of this ...study included the extraction and analysis of the volatile compounds by performing a supercritical CO2 (SC-CO2) extraction under different operating pressure conditions (100 and 300 bar). The analysis of volatile compounds of the obtained extracts was conducted by gas chromatography-mass spectrometry (GC-MS), and limonene was found to be the dominant volatile component (13.16% at 100 bar; 30.65% at 300 bar). After SC-CO2 treatment, the exhausted citrus peel waste enriched with bioactive compounds was subjected to subcritical water extraction (SWE) in a wide temperature range (130–220 °C) using different solvent-solid ratio (10–30 mL/g) in time periods from 5 to 15 min, in order to obtain bioflavonoids. Identification and quantification of present bioflavonoids was conducted by high-performance liquid chromatography with a with a diode array detector (HPLC), and hesperidin (0.16–15.07 mg/g) was determined as the most abundant flavanon in mandarin peel with other polyphenolic compounds that were possible by-products of thermal degradation. At higher temperatures, the presence of 5-hydroxymethylfurfural (5-HMF) and chlorogenic acid were detected. Antiradical activity and total phenolic content in the extracts were determined using spectrophotometric methods, while the process optimization was performed by response surface methodology (RSM).
Ultrasound-assisted extraction (UAE) of fucoxanthin and total pigment content was performed from brown, red and green macroalgal species (
Fucus virsoides
,
Amphiroa rigida
and
Codium bursa
) from ...the Adriatic Sea under different experimental conditions of time (15, 30 and 45 min), temperature (30, 50 and 70 °C) and solvent:solid ratio (10, 20 and 30 mL g
−1
). UAE was evaluated to determine the conditions influence on fucoxanthin yield (dominant pigment). The results showed that brown macroalga
F. virsoides
contained the highest fucoxanthin content (1.19–1.90 mg g
−1
dry extract), followed by red macroalga
A. rigida
(0.29–0.90 mg g
−1
dry extract) and green macroalga
C. bursa
(0.07–0.43 mg g
−1
dry extract). Additionally, total concentrations of pigments (chlorophyll
a
, chlorophyll
b
and carotenoids) were determined by spectrophotometric analysis. Significant dependence on the applied extraction conditions for fucoxanthin and total pigments yields was revealed by the analysis of variance for the response surface models. Accordingly, the results showed differences for each macroalgal species in terms of the optimal UAE parameters. It can be concluded that UAE is successful method for the extraction of fucoxanthin from different macroalgal species, but the extraction optimization is crucial.
Graphical abstract
The focus of present study is on
collected from the Adriatic Sea.
volatiles were identified by gas chromatography and mass spectrometry (GC-FID; GC-MS) after headspace solid-phase microextraction ...(HS-SPME), hydrodistillation (HD), and supercritical CO₂ extraction (SC-CO₂). The headspace composition of dried (HS-D) and fresh (HS-F)
was remarkably different. Dimethyl sulfide, the major HS-F compound was present in HS-D only as a minor constituent and heptadecane percentage was raised in HS-D. The distillate of fresh
contained heptadecane and docosane among the major compounds. After air-drying, a significantly different composition of the volatile oil was obtained with (
)-phytol as the predominant compound. It was also found in SC-CO₂ extract of freeze-dried
(FD-CB) as the major constituent. Loliolide (3.51%) was only identified in SC-CO₂ extract. Fatty acids were determined from FD-CB after derivatisation as methyl esters by GC-FID. The most dominant acids were palmitic (25.4%), oleic (36.5%), linoleic (11.6%), and stearic (9.0%). FD-CB H₂O extract exhibited better antifungal effects against
spp., while dimethyl sulfoxide (DMSO) extract was better for the inhibition of
, and
spp. The extracts showed relatively good antifungal activity, especially against
(for DMSO extract MIC
was at 50 µg/mL).
Natural products are increasingly in demand in dermatology and cosmetology. In the present study, highly valuable supercritical CO2 (sCO2) extracts rich in bioactive compounds with antiradical and ...antibacterial activity were obtained from the inflorescences of industrial hemp. Volatile compounds were analyzed by gas chromatography in tandem with mass spectrometry (GC-MS), while cannabinoids were determined by high performance liquid chromatography (HPLC-DAD). Extraction yields varied from 0.75 to 8.83%, depending on the pressure and temperature applied. The extract obtained at 320 bar and 40 °C with the highest content (305.8 µg mg−1) of cannabidiolic acid (CBDA) showed the best antiradical properties. All tested extract concentrations from 10.42 µg mL−1 to 66.03 µg mL−1 possessed inhibitory activities against E. coli, P. aeruginosa, B. subtilis, and S. aureus. The sCO2 extract with the highest content of cannabidiol (CBD) and rich in α-pinene, β-pinene, β-myrcene, and limonene was the most effective. The optimal conditions for sCO2 extraction of cannabinoids and volatile terpenes from industrial hemp were determined. The temperature of 60 °C proved to be optimal for all responses studied, while the pressure showed a different effect depending on the compounds targeted. A low pressure of 131.2 bar was optimal for the extraction of monoterpenes, while extracts rich in sesquiterpenes were obtained at 319.7 bar. A high pressure of 284.78 bar was optimal for the extraction of CBD.
Six medicinal plants
(Roth) G. Don,
L.,
L.,
L.,
L., and
L. were used. The aim of the study was to compare their extracts obtained by Soxhlet (hexane) extraction, maceration with ethanol (EtOH), and ...supercritical CO₂ extraction (SC-CO₂) targeted on coumarin content (by high performance liquid chromatography with ultraviolet detection, HPLC-UV), 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) scavenging capacity, and total phenols (TPs) content (by Folin-Ciocalteu assay). The highest extraction yields were obtained by EtOH, followed by hexane and SC-CO₂. The highest coumarin content (316.37 mg/100 g) was found in
EtOH extracts, but its SC-CO₂ extraction yield was very low for further investigation. Coumarin was also found in SC-CO₂ extracts of
,
,
, and
. EtOH extracts of all plants exhibited the highest DPPH scavenging capacity. SC-CO₂ extracts exhibited antiradical capacity similar to hexane extracts, while
SC-CO₂ extracts were the most potent (95.7%). EtOH extracts contained the most TPs (up to 132.1 mg gallic acid equivalents (GAE)/g from
) in comparison to hexane or SC-CO₂ extracts. TPs content was highly correlated to the DPPH scavenging capacity of the extracts. The results indicate that for comprehensive screening of different medicinal plants, various extraction techniques should be used in order to get a better insight into their components content or antiradical capacity.
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•Integrated extraction pathway applied for orange peel waste utilization.•Supercritical extract of orange peel is a good source of fatty acids and coumarins.•Ultrasound-assisted ...extracts of orange peel represents a good source of polyphenols.•In silico evaluation of obtained extracts are showing a wide range of bioactivities.
This study is focused on the investigation of the new ways of valorization and maximal utilisation of the fruit dust obtained from the orange peel during industrial processing in the filter tea production. Therefore, the possibility of the integration of two attractive “green” extraction methods, CO2-assisted extraction and ultrasound-assisted extraction (UAE), were investigated. In the first step to produce herbal extracts, supercritical carbon dioxide (Sc-CO2) extraction of the orange peel dust (OPD) was applied in the pressure range of 10–30 MPa. The second step was UAE of the OPD remaining after the Sc-CO2 extraction, with varying sonication amplitudes (20–100%). Gas chromatography combined with mass spectrometry was used for the chemical characterization of Sc-CO2 extracts. Among the valuable volatile compounds, the most abundant are linoleic (31.11–41.47%) and hexadecanoic (15.22–20.58%) acid, osthol (4.53–5.42%), and 7-methoxy-8-(2-oxo-3-methylbutyl) coumarin (12.65–15.45%). Extracts obtained by UAE were analyzed by HPLC, where the dominant compounds were identified as hesperidin (848–900.24 µg/ml), narirutin (16.70–18.16 µg/ml), naringin (771.45––830.39 µg/ml) and rutin (47.53–104.40 µg/ml). Finally, the in silico testing was performed to identify pharmacologically the most valuable bioactive compounds in the extracts, and to enable screening of the possible pharmacological effect and applications of the obtained.
Freeze drying and spray drying techniques were evaluated for encapsulation of pure hesperidin and hesperidin from citrus peel extract in Maltodextrin and Gum Arabic in order to improve hesperidin ...stability and solubility. Physicochemical and structural properties of the microcapsules were determined and compared with the standardized high-purity hesperidin. Solubility of obtained microcapsules, defined by high WAI (0.202–0.697 g/g), WSI (88.02–99.746 %) and OAI (2.174–4.56 g/g), caused mainly by the amorphization of hesperidin structure was significantly improved. It was also confirmed with PXRD analyses. Microcapsules were of light colour, characterized by colour changes in the range from 12.57 to 47.49 and high whiteness index (64.12–94.45). The beneficial effect of encapsulation techniques is evident in flow properties where the Hausner ratio was in the range of 1.023–1.304 and Carr's index in the range of 2.26–23.273 %. Obtained microcapsules had satisfying hesperidin retention with encapsulation efficiency from 7.56 to 65.29 % and thermal stability above 110 °C. The best results were obtained for pure hesperidin encapsulated with freeze drying, satisfying results were obtained for citrus peel extract encapsulated in maltodextrin using spray drying. Obtained results indicate that the encapsulation of hesperidin can protect its bioactivities from environmental conditions and improve its solubility and flow properties, hence increasing its functional capabilities as pharmaceutical and cosmetic ingredients or additives.
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•Two encapsulation techniques (spray drying and freeze-drying) can be used for the encapsulation of hesperidin.•Maltodextrin and Gum Arabic can be coating materials of hesperidin microcapsules.•Solubility and flow properties of hesperidin microparticles are improved due to encapsulation.•Hesperidin from citrus peel extract may be an alternative for hesperidin drug delivery systems.
In continuation of our efforts to fully utilize eggshell waste (ESW), here we report the possibility of ESW transformation to calcium chloride (CaCl
) anhydride of food-grade additive purity and ...eggshell membranes (ESMs) as potential enzyme immobilization carriers. ESW chemical transformation by 5% (w/v) hydrochloric acid to CaCl
solution and ESM completely devoid of the remnants of ESW calcium carbonate was performed in the constructed 15 L batch reactor during 4 h at room temperature, followed by separation of ESM from CaCl
solution by filtration. ESW-derived CaCl
solution containing the excess hydrochloric acid was neutralized by adding calcium hydroxide, concentrated to approximately 1/8th of volume, and spray dried. Separated ESM was washed with water and acetone, dried, and ground to a size of less than 0.5 mm. The ESW transformation process produced 102.42 ± 3.31 g of CaCl
anhydrous and 2.48 ± 0.28 g of ESM per 100 g of ESW dry matter. ESW-derived CaCl
fulfilled all criteria for food-grade additive, while obtained ESM showed their suitability for
lipase immobilization by adsorption.
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