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1.
The extraction procedures (solid/liquid SPE and liquid/liquid LLE) and HPLC separation and quantification methods of polyphenolic compounds have been checked in virgin olive oils in order to explain the differences in content reported in the literature. The work has been carried out on oils prepared from one cultivar and produced under the same protocol. The extraction methods are practically equivalent, but the SPE technique is more favorable because it is faster and simpler. It has been proved that the chromatographic features and the method of chemical expression of the concentrations may greatly affect the final values. Thus, under the same analytical method, the total concentration values of polyphenols of the same oil show variations from 18% to 80%, according to the formality of expression as gallic acid, caffeic acid, or tyrosol equivalents. The role of the nature and spectrophotometric features of the phenols and of the internal standard is also discussed, and it was found to be an important source of reported variation. A gradient separation with an eluent mixture acetonitrile-sulfuric acid (0.1 mol/L), detection at 225 nm, and quantitative calculation of polyphenolic compounds in oils (expressed as tyrosol equivalents, THY(eq)) is proposed.  相似文献   

2.
A method for the multiresidue determination of 35 pesticides (30 insecticides and five herbicides) in olive oil by gas chromatography (GC) is described. Three liquid-liquid extraction (LLE) procedures based on (i) partition of pesticides between acetonitrile (ACN) and oil solution in n-hexane, (ii) partition of pesticides between saturated ACN with n-hexane and oil solution in n-hexane saturated with ACN, and (iii) partition of pesticides between ACN and oil were tested for the optimization of the highest pesticide recoveries with the lowest oil residue in the final extracts. Experimental tests were preformed in order to study the efficiency of different clean up procedures with N-Alumina, Florisil, C18, and ENVI-Carb solid-phase extraction (SPE) cartridges for the compounds analyzed by GC-nitrogen phosphorus detection. A second step of clean up was also performed for the compounds analyzed by GC-electron capture detection (ECD), by using phenyl-bonded silica (Ph), diol-bonded silica (Diol), cyanopropyl-bonded silica (CN), and amino propyl-bonded silica (NH2) SPE cartridges. LLE of the oil solution in hexane with ACN followed by an ENVI-Carb SPE clean up of the extract gave the best results for all target compounds. The ACN extract was additionally cleaned through a Diol-SPE cartridge for the determination of pesticides analyzed mainly by GC-ECD. Pesticide recoveries form virgin olive oil spiked with 20, 100, and 500 microg/kg concentrations of pesticides ranged from 70.9 to 107.4%. The proposed method featured good sensitivity, pesticide quantification limits were low enough, and the precision, expressed as relative standard deviation, ranged from 2.4 to 12.0%. The proposed method was applied successfully for the residue determination of the selected pesticides in commercial olive oil samples.  相似文献   

3.
This study presents the phenolic compounds profile of commercial Cornicabra virgin olive oils from five successive crop seasons (1995/1996 to 1999/2000; n = 97), determined by solid phase extraction reversed phase high-performance liquid chromatography (SPE RP-HPLC), and its relationship with oxidative stability, processing conditions, and a preliminary study on variety classification. The median of total phenols content was 38 ppm (as syringic acid), although a wide range was observed, from 11 to 76 ppm. The main phenols found were the dialdehydic form of elenolic acid linked to tyrosol (p-HPEA-EDA; 9 +/- 7 ppm, as median and interquartile range), oleuropein aglycon (8 +/- 6 ppm), and the dialdehydic form of elenolic acid linked to hydroxytyrosol (3,4-DHPEA-EDA; 5 +/- 8 ppm). In many cases the correlation with oxidative stability was higher when the sum of the dialdehydic form of elenolic acid linked to hydroxytyrosol (3,4-DHPEA-EDA) and oleuropein aglycon (r (2) = 0.91-0.96) or the sum of these two and hydroxytyrosol (r (2) = 0.90-0.97) was considered than was observed with HPLC total phenols (r (2)= 0.91-0.95) and especially with colorimetric determination of total polyphenols and o-diphenols (r (2) = 0.77-0.95 and 0.78-0.92, respectively). 3,4-DHPEA-EDA, p-HPEA-EDA, the aglycons of oleuropein and ligstroside, and HPLC total phenols content presented highly significant differences (p = 0.001-0.010) with respect to the dual- and triple-phase extraction systems used, whereas colorimetric total polyphenols content did not (p = 0.348) and o-diphenols showed a much lower significant difference (p = 0.031). The five variables that most satisfactorily classified the principal commercial Spanish virgin olive oil varieties were 1-acetoxypinoresinol, 4-(acetoxyethyl)-1,2-dihydroxybenzene (3,4-DHPEA-AC), ligstroside aglycon, p-HPEA-EDA, and RT 43.3 contents.  相似文献   

4.
A simple and precise analytical method for the determination of hydroxy pentacyclic triterpene acids (HPTAs) in vegetable oils was developed. The acidic fraction was isolated by solid-phase extraction using bonded aminopropyl cartridges, and the extract was silylated and analyzed by gas chromatography. Repeatability and recovery of the method were determined. In virgin olive oils, similar amounts of oleanolic (3beta-hydroxyolean-12-en-28-oic) and maslinic (2alpha,3beta-dihydroxyolean-12-ene-28oic) acids and traces of ursolic (3beta-hydroxyurs-12-en-28-oic) acid were found. The main factor affecting HPTA concentration was the oil quality since that increases as the quality decreases, while olive variety, olive ripeness, and oil extraction system had less influence. In crude olive pomace oils, the concentrations were very much higher than in virgin olive oils. During refining processes, total or significant losses of HPTAs were observed. Esterified derivatives of HPTAs were not found.  相似文献   

5.
A simple and reproducible method for qualitative and quantitative analysis of phenolic compounds in virgin olive oils by solid-phase extraction (SPE), high performance liquid chromatography with diode array detector (HPLC-DAD), and HPLC-mass spectrometry (MS) in tandem mode was developed. The polar fraction was obtained from samples of three different virgin olive oils. Detection and quantification were performed at 280, 240, and 320 nm. For identification purposes, HPLC-MS/MS was equipped with turbo ion spray source in the negative-ion mode. Twenty compounds of twenty-three detected and quantified were characterized. The method showed satisfactory linearity (r > 0.99), good recovery, satisfactory precision, and appropriate limits of detection (LOD) and quantification (LOQ).  相似文献   

6.
A simple and precise analytical method was developed for the simultaneous determination of squalene and methyl, ethyl, propyl, and butyl esters of fatty acids present in olive and olive pomace oils. A fraction containing squalene and fatty acid alkyl esters was isolated from the oil by solid phase extraction on silica gel cartridges and quantitatively analyzed by gas chromatography. A modification of the procedure allowed the isolation of squalene and esters separately. Repeatability and recovery of the method were good. The method was applied to extra and lampant virgin olive oil categories and also to oils obtained from olive pomace by second centrifugation and solvent extraction. Extra virgin olive oils contained low amounts of fatty acid methyl and ethyl esters, while oils obtained from altered olive or olive pomace showed high concentrations of fatty acid alkyl esters, mainly ethyl esters. Correlation between oil acidity and ethyl esters concentration was poor.  相似文献   

7.
Capillary electrophoresis (CE) can be effectively used as a fast screening tool to obtain qualitative and semiquantitative information about simple and complex phenolic compounds of extra virgin olive oil. Three simple phenols (tyrosol, hydroxytyrosol, and vanillic acid), a secoiridoid derivative (deacetoxy oleuropein aglycon), and two lignans (pinoresinol and acetoxypinoresinol) were detected as the main compounds in extra virgin olive oils by high-performance liquid chromatography (HPLC) and capillary zone electrophoresis (CZE). Spectrophotometric indices, radical scavenging activity, and oxidative stability of extra virgin olive oil samples obtained from olives hand-picked at different ripening degrees were statistically correlated with the CZE and HPLC quantification. The concentration of phenols in extra virgin olive oil decreased with ripeness of olive fruits. The high correlations found between CZE and the other analytical results indicate that CE can be applied as a rapid and reliable tool to routinely determine phenolic compounds in extra virgin olive oils.  相似文献   

8.
Extraction methods to determine olive oil phenols are not exhaustive. A procedure to test their effectiveness, based on the treatment of the extracted oil with 2 N HCl followed by analysis of phenols in the aqueous phase, has been developed. It was concluded, using this test, that 15-40% of phenols remained unextracted when the liquid/liquid extraction method with 80% methanol was applied. Solid phase extraction (C(18) cartridge) succeeded in retaining most of the phenols in the cartridge, but the recovery yield from the sorbent material was low. However, a new extraction method, based on the use of N,N-dimethylformamide (DMF) as an extraction solvent, achieved a complete extraction of phenols from oils. The proposed method requires a lower amount of oil, solvents, energy, and labor than the traditional ones. Because of the low concentration of phenols in the DMF extract, the highly sensitive electrochemical detector (EC) technique was studied. All of the phenols detected by the traditional UV detectors were also detected by EC using a coulometric array system. A rapid and complete analytical methodology of phenols in olive oil has been proposed based on coupling DMF extraction and EC detection.  相似文献   

9.
A high-performance liquid chromatography (HPLC) method was developed to quantitatively analyze oleocanthal in extra virgin olive oils. Oleocanthal, a deacetoxy ligstroside aglycone, is known to be responsible for the back of the throat irritation of olive oils and to have probated antiinflamatory activity. Oleocanthal was isolated from small amounts of olive oil sample (1 g) by liquid-liquid extraction. Hexane-acetonitrile was found to be the best solvent system to extract oleocanthal from the oil matrix. The solvent extract was analyzed by reversed-phase HPLC with UV detection at 278 nm. Chromatogaphic separation of oleocanthal from other extracted compounds and of the two geometric isomers of oleocanthal was achieved by an elution gradient with acetonitrile and water. Both the external standard calibration curve and the internal standard calibration curve were established, and quantitation using both calibration curves gave essentially the same result. The reproducibility (RSD = 4.7%), recovery (> 95%), and limit of quantitation (< 1 microg/g) were also determined. Concentrations of oleacanthal in 10 selected throat-burning extra virgin olive oils were determined using the method (ranged from 22 to 190 microg/g) with external standard calibration.  相似文献   

10.
Fatty acid esters of 3-(N-phenylamino)-1,2-propanediol are currently considered the best chemical markers of toxic oils related to the Spanish toxic oil syndrome. Recent research in this area has undertaken the exhaustive and quantitative characterization of these compounds in oils collected during the epidemic outbreak. Current methods developed in this laboratory are based on solid phase extraction (SPE) using SCX cartridges followed by HPLC-APCI/MS/MS quantification. To circumvent the long and tedious extraction procedure, the SPE protocol was adapted for automatic extraction and the problems derived from the use of the immiscible solvents required for the SCX extraction were solved. Linearity of the analytical method was found in the same range as for the manual method. Extraction recoveries were 87 and 75% for 2-hydroxy-3-(N-phenylamino)propyl linoleate and 2-(linoleyloxy)-3-(N-phenylamino)propyl linoleate, respectively, and the corresponding coefficients of variation were approximately 1%, greatly improving reproducibility over manual procedures.  相似文献   

11.
Many epidemiological studies suggest that vegetable oils and especially olive oil present a protective effect against atherosclerosis. In this study, total lipids (TL) of Greek olive oils and seed oils of four kinds, namely, soybean, corn, sunflower, and sesame oil, were separated into total polar lipids (TPL) and total neutral lipids (TNL) via a novel extraction procedure. TPL and TNL of olive oil were fractionated by HPLC for further study. Each lipid fraction from HPLC separation along with TL, TPL, and TNL lipid samples from oils were tested in vitro for their capacity to induce or to inhibit washed rabbit platelet aggregation. Comparison between olive and seed oils supports the superiority of olive oil as high levels of platelet activating factor (PAF) antagonists have been detected, mainly in TPL. In addition, the structure of the most active fraction from olive oil was elucidated, as a glycerol-glycolipid. Because it has already been reported that PAF plays a pivotal role in atherogenesis, the existence of PAF agonists and antagonists in vegetable oils may explain their protective role against atherosclerosis.  相似文献   

12.
A liquid-liquid extraction method to enrich edible oils--olive, sunflower, and soy oils--with phenols from olive leaf extracts is proposed. After microwave assistance to remove the phenols from three varieties of olive leaves, concentrations in the extracts between 12921 and 5173 mg/L of oleuropein, between 488 and 192 mg/L of apigenin-7-glucoside, between 444 and 219 mg/L of luteolin-7-glucoside, and between 501 and 213 mg/L of verbascoside were obtained, which clearly depended on the target variety. After optimization of the liquid-liquid extraction step, the concentrations in oils were 442, 162, and 164 mg/L of oleuropein, respectively, which were also enriched in apigenin-7-glucoside (between 8 and 15 mg/L, depending of the oil), lutelin-7-glucoside (between 11 and 12 mg/L), and verbascoside (between 11 and 13 mg/L). The oil-extract distribution factor of these compounds was also calculated for all olive leaf varieties and edible oils using different extracts concentrations and also different oil-extract volume ratios. Thus, a door is open to enrichment of any oil with olive phenols at preset concentrations using extracts preconcentrated as required and taking into account the distribution factor of the target compounds between the oil and the extracts.  相似文献   

13.
Phenolic compounds in Spanish virgin olive oils were characterized by HPLC. Simple phenols such as hydroxytyrosol, tyrosol, vanillic acid, p-coumaric acid, ferulic acid, and vanillin were found in most of the oils. The flavonoids apigenin and luteolin were also found in most of the oils. The dialdehydic form of elenolic acid linked to tyrosol and hydroxytyrosol was also detected, as were oleuropein and ligstroside aglycons. The structure of a new compound was elucidated by MS and NMR as being that of 4-(acetoxyethyl)-1,2-dihydroxybenzene. Changes of phenolic compounds in virgin olive oils with maturation of fruits were also studied. Hydroxytyrosol, tyrosol, and luteolin increased their concentration in oils with maturation of fruits. On the contrary, glucoside aglycons diminished their concentration with maturation. No clear tendency was observed for the rest of the phenolic compounds identified.  相似文献   

14.
Phenolic extracts from olive tree leaves and olive pomace were used to enrich refined oils (namely, maize, soy, high-oleic sunflower, sunflower, olive, and rapeseed oils) at two concentration levels (200 and 400 μg/mL, expressed as gallic acid). The concentration of characteristic olive phenols in these extracts together with the lipidic composition of the oils to be enriched influenced the mass transfer of the target antioxidants, which conferred additional stability and quality parameters to the oils as a result. In general, all of the oils experienced either a noticeable or dramatic improvement of their quality-stability parameters (e.g., peroxide index and Rancimat) as compared with their nonenriched counterparts. The enriched oils were also compared with extra virgin olive oil with a natural content in phenols of 400 μg/mL. The healthy properties of these phenols and the scarce or nil prices of the raw materials used can convert oils in supplemented foods or even nutraceuticals.  相似文献   

15.
The most abundant phenolic compounds in olive oils are the phenethyl alcohols hydroxytyrosol and tyrosol. An optimized method to quantify the total concentration of these substances in olive oils has been described. It consists of the acid hydrolysis of the aglycons and the extraction of phenethyl alcohols with a 2 M HCl solution. Recovery of the phenethyl alcohols from oils was very high (<1% remained in the extracted oils), and the limits of quantification (LOQ) were 0.8 and 1.4 mg/kg for hydroxytyrosol and tyrosol, respectively. Precision values, both intraday and interday, remained below 3% for both compounds. The final optimized method allowed for the analysis of several types of commercial olive oils to evaluate their hydroxytyrosol and tyrosol contents. The results show that this method is simple, robust, and reliable for a routine analysis of the total concentration of these substances in olive oils.  相似文献   

16.
Besides affecting the oil's sensorial characteristics, the presence of herbs and spices has an impact on the nutritional value of the flavored oils. The aim of the study was to develop a new product based on the phenol-enrichment of a virgin olive oil with both its own phenolic compounds (secoiridoid derivatives) plus additional complementary phenols from thyme (flavonoids). We studied the effect of the addition of phenolic extracts (olive cake and thyme) on phenolic composition, oxidative stability, antioxidant activity, and bitter sensory attribute of olive oils. Results showed that flavonoids from thyme appeared to have higher transference ratios (average 89.7%) from the phenolic extract to oil, whereas secoiridoids from olive presented lower transference ratios (average 35.3%). The bitter sensory attribute of the phenol-enriched oils diminished with an increase of the concentration of phenols from thyme, which might denote an improvement in the consumer acceptance.  相似文献   

17.
A sensitive and reliable method was developed and validated for trace determination of sulfonylurea herbicides residues in cereals (wheat, rice, and corn) by liquid chromatography-tandem mass spectrometry. The selected analytes were ethoxysulfuron, ethametsulfuron-methyl, bensulfuron-methyl, chlorimuron-ethyl, pyrazosulfuron-ethyl, and cyclosulfamuron. In this work, the extraction procedure was performed by using a mixture solvent of phosphate buffer (pH 9.5)/acetonitrile (8:2, v/v) as the extraction solvent and then was cleaned up by using Spe-ed C18/18% SPE cartridges, providing good recoveries for all of the tested analytes and with no matrix effects affecting method accuracy. The limits of detection for the studied analytes in cereal samples were between 0.043 and 0.23 μg kg(-1), and the limits of quantification were between 0.14 and 0.77 μg kg(-1), lower in all cases than the maximum residue limits permitted by the European Union for this kind of food. The developed methodology has demonstrated its suitability for the monitoring of these residues in cereal samples with high sensitivity, precision, and satisfactory recoveries.  相似文献   

18.
Bitterness and pungency, sensory quality attributes of virgin olive oil, are related to the presence of phenolic compounds. Fast and reliable alternatives for the evaluation of sensory attributes and phenolic content are desirable, as sensory and traditional analytical methods are time-consuming and expensive. In this study, two amperometric enzyme-based biosensors (employing tyrosinase or peroxidase) for rapid measurement of polar phenolics of olive oil were tested. The biosensor was constructed using disposable screen-printed carbon electrodes with the enzyme as biorecognition element. The sensor was coupled with a simple extraction procedure and optimized for use in flow injection analysis. The performance of the biosensor was assessed by measuring a set of virgin olive oils and comparing the results with data obtained by the reference HPLC method and sensory scores. The correlations between the tyrosinase- and peroxidase-based biosensors and phenolic content in the samples were high (r = 0.82 and 0.87, respectively), which, together with a good repeatability (rsd = 6%), suggests that these biosensors may represent a promising tool in the analysis of the total content of phenolics in virgin olive oils. The correlation with sensory quality attributes of virgin olive oil was lower, which illustrates the complexity of sensory perception. The two biosensors possessed different specificities toward different groups of phenolics, affecting bitterness and pungency prediction. The peroxidase-based biosensor showed a significant correlation (r = 0.66) with pungency.  相似文献   

19.
Hydrophilic phenols are the most abundant natural antioxidants of virgin olive oil (VOO), in which tocopherols and carotenes are also present. The prevalent classes of hydrophilic phenols found in VOO are phenyl alcohols, phenolic acids, secoiridoids such as the dialdehydic form of decarboxymethyl elenolic acid linked to (3,4-dihydroxyphenyl)ethanol or (p-hydroxypheny1)ethanol (3,4-DHPEA-EDA or p-HPEA-EDA) and an isomer of the oleuropein aglycon (3,4-DHPEA-EA), lignans such as (+)-1-acetoxypinoresinol and (+)-pinoresinol, and flavonoids. A new method for the analysis of VOO hydrophilic phenols by direct injection in high-performance liquid chromatography (HPLC) with the use of a fluorescence detector (FLD) has been proposed and compared with the traditional liquid-liquid extraction technique followed by the HPLC analysis utilizing a diode array detector (DAD) and a FLD. Results show that the most important classes of phenolic compounds occurring in VOO can be evaluated using HPLC direct injection. The efficiency of the new method, as compared to the liquid-liquid extraction, was higher to quantify phenyl alcohols, lignans, and 3,4-DHPEA-EA and lower for the evaluation of 3,4-DHPEA-EDA and p-HPEA-EDA.  相似文献   

20.
A multicolumn solid-phase extraction cleanup for the determination of organophosphorus (OP) and organochlorine (OC) pesticides plus PCB congeners in virgin olive oil is presented. The method involves dissolution of the olive oil in hexane, followed by a cleanup system using a diatomaceous earth column (Extrelut-QE) with reversed (C(18)) and normal (alumina) phase SPE columns. Determination of OPs was by GC-NPD, while the OCs and PCBs were analyzed using GC-ECD. Recovery assays for OPs varied from 81.7% to 105.3%, for OCs ranged between 74.3% and 99.4%, while for PCBs were from 60.1% to 119.2%. Quantitation limits ranged from 10 to 25 microg/kg olive oil for OPs, and from 1 to 6 microg/kg olive oil for OCs and PCBs. In the case of positive samples, the confirmation of pesticide identity was performed by ion-trap GC-MS/MS. The applicability of the method was assayed with 19 virgin olive oil samples collected from different olive mills of Aragón (Spain). Only one OP pesticide (acephate) was detected in one sample at a concentration of 10 microg/kg. Organochlorine pesticides were found in 5-47% of samples at very low levels ranging from 1.5 to 5.2 microg/kg. PCBs were found in 20-90% of samples, showing concentrations between 2.3 and 17.3 microg/kg.  相似文献   

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