Virgin olive oils (VOOs) obtained from the fruits of Croatian autochthonous varieties Mašnjača and Krvavica were extensively characterized for the first time. Investigated oils were compared with the oil obtained from Italian variety Leccino, grown and processed under the same conditions. Headspace volatile profile, tocopherols, chlorophylls, carotenoids and total phenolic content, peroxide value, % acidity, K 232 , K 270 as well as antioxidant activity (DPPH) of the oils' hydrophilic fractions (HFs) including their phenolic composition were assessed by means of HS-SPME/GC-MS, HPLC-FL, HPLC-DAD and spectrophotometric methods, respectively. Most of the studied quality parameters varied between the cultivars. The main volatile compounds detected in all tested olive oils were the C6 compounds derived from polyunsaturated fatty acids through the lipoxygenase pathway. Krvavica oil was characterized by hexanal (8.8%-9.4%). Leccino oil contained the highest percentage of (E)-hex-2-enal (73.4%-74.0%), whereas 882(Z)-hex-3-enal (21.9%-25.0%) and (E)-hex-2-enal (27.6%-28.9%) dominated in Mašnjača oil. Leccino oil contained the highest amount of tocopherols (312.4 mg/kg), chlorophylls (7.3 mg/kg), carotenoids (4.2 mg/kg) and total phenols (246.6 mg/kg). The HF of Leccino oil showed the highest antioxidant capacity (1.3 mmol TEAC/kg), while the HFs of Mašnjača and Krvavica oils exhibited the activity of 0.5 mmol TEAC/kg.
Volatile organic compounds of Amorpha fruticosa honey samples were isolated by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE), followed by gas chromatography and mass spectrometry analyses (GC, GC-MS), in order to obtain complementary data for overall characterization of the honey aroma. The headspace of the honey was dominated by 2-phenylethanol (38.3–58.4%), while other major compounds were trans- and cis-linalool oxides, benzaldehyde and benzyl alcohol. 2‑Phenylethanol (10.5–16.8%) and methyl syringate (5.8–8.2%) were the major compounds of ultrasonic solvent extracts, with an array of small percentages of linalool, benzene and benzoic acid derivatives, aliphatic hydrocarbons and alcohols, furan derivatives and others. The scavenging ability of the series of concentrations of the honey ultrasonic solvent extracts and the corresponding honey samples was tested by a DPPH (1,1-diphenyl-2-picrylhydrazyl) assay. Approximately 25 times lower concentration ranges (up to 2 g/L) of the extracts exhibited significantly higher free radical scavenging potential with respect to the honey samples.
Samples of unifloral sulla (Hedysarum coronarum L.) honey from Sardinia (Italy) were analysed. To investigate the chemical composition of the honey volatiles two solvent systems were used for ultrasonic solvent extraction (USE): 1) a 1:2 (v/v) pentane and diethyl ether mixture and 2) dichloromethane. All the extracts were analysed by GC and GC/MS. These procedures have permitted the identification of 56 compounds that include norisoprenoids, benzene derivatives, aliphatic compounds and Maillard reaction products. Norisoprenoids were the major compounds in both extracts, dominated by vomifoliol (5.3-11.2%; 9.6-14.0%) followed by minor percentages of other norisoprenoids such as α-isophorone, 4-ketoisophorone, 3-oxo-α-ionol or 3-oxo-α-ionone. Other abundant single compounds in the extracts were 3-hydroxy-4-phenylbutan-2-one (0.8-5.4%; 0.6-5.7%) and methyl syringate (3.0-5.7%; 2.2-4.1%). The composition of the volatiles and semi-volatiles in the obtained extracts suggests that sulla honey is quite distinctive relative to the other honeys that have been chemically studied by GC/MS, but no specific markers of the honey botanical origin were found.
An ancient organic residue was collected from the bottom of a Greco-Italian amphora found in the Adriatic Sea and investigated by direct GC and GC-MS analysis. The headspace composition was determined by HS-SPME using: (1) DVB/CAR/PDMS and (2) PDMS/DVB fibres. Higher percentages of benzene derivatives, monoterpenes and other low-molecular aliphatic compounds were obtained by method (1) in contrast to higher percentage of naphthalene and phenanthrene derivatives found by method (2). In comparison with the composition of pine resin, it is more likely that the found low-molecular aliphatic alcohols, acids, esters and carbonyls with 2-phenylethanol were trapped and preserved within the organic residue from stored wine – the amphora’s originally content. Semi-volatile diterpenes methyl dehydroabietate (33.6%) and retene (24.1%) were dominant in the residue CH2Cl2 solution. Other abundant compounds were 1,4-dimethoxyphenanthrene (6.8%) as well as other naphthalene and/or phenanthrene derivatives [7-(1-methylethyl)-1,4a-dimethyl-1,2,3,4,4a,9,10,10a-octahydronaphthalene, 7-(1-methylethyl)-1,4a-dimethyl-2,3,4,4a,9,10-hexahydrophenanthrene, 7-(1-methylethyl)-1,4a-dimethyl-1,2,3,4,4a,9,10,10a-octahydro-phenanthrene, 3,6-dimethylphenanthrene and 2,3,5-trimethylphenanthrene]. Possible sources and formation pathways of the major compounds in the residue were discussed.
Virgin olive oils from the fruits of Croatian autochthonous varieties Oblica, Lastovka and Levantinka were characterized for the first time. Headspace volatiles were analyzed by HS-SPME/GC-FID/MS. The main volatiles were C6 compounds. The most abundant was (E)-hex-2-enal (62.60%-69.20%). (Z)-Hex-3-enal was not found in Lastovka oil, while Levantinka oil did not contain hexanal. Tocopherols, chlorophylls and carotenoids were determined by HPLC-FL. Levantinka oil was characterized by the highest α-tocopherol level (222.00 mg/kg). Total phenolic contents (TPs), as well as antioxidant activity (DPPH assay) of the oils hydrophilic fractions (HFs) were assessed by spectroscopic methods. The antioxidant activity of Oblica oil HF was the most pronounced (0.91 mmol TEAC/kg) and the HF contained the highest TPs amount (212.21 mg/kg). HFs phenolic composition was determined by HPLC-DAD. The main identified phenols were secoiridoids dominated in Oblica oil: decarboxymethyl ligstroside aglycone (p-HPEA-EDA up to 158.5 mg/kg), oleuropein aglycone (3,4-HPEA-EA up to 96.4 mg/kg) and decarboxymethyl oleuropein aglycon (3,4-DHPEA-EDA up to 93.5 mg/kg).
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