Extracción en fase sólida: Aplicaciones al análisis cromatográfico de aceites y grasas vegetales

Applications of solid-phase extraction for the isolation of certain lipid classes prior to chromatographic analysis are given. More information was found for sterols and related compounds, polar phenols and contaminants such as polycyclic aromatic hydrocarbons. Detailed analytical protocols are presented and discussed in many cases.Se analizan las aplicaciones de la extracción en fase sólida para el aislamiento de ciertos lípidos previamente al análisis cromatográfico. La mayor parte de la información se refiere a los esteroles y compuestos relacionados, fenoles polares y contaminantes como los hidrocarburos aromáticos policíclicos. Se muestran y discuten numerosos protocolos analíticos en detalle

In house validated UHPLC protocol for the determination of the total hydroxytyrosol and tyrosol content in virgin olive oil fit for the purpose of the health claim introduced by the EC Regulation 432/2012 for \u201cOlive oil polyphenols\u201d

An ongoing challenge in olive oil analytics is the development of a reliable procedure that can draw the consensus of all interested parties regarding the quantification of concentrations above the required minimum value of 5 mg of bioactive "olive oil polyphenols" per 20 g of the oil, to fulfill the health claim introduced by the European Commission (EC) Regulation 432/2012. An in-house validated ultra-high performance liquid chromatography (UHPLC) protocol fit for this purpose is proposed. It relies on quantification of the total hydroxytyrsol (Htyr) and tyrosol (Tyr) content in the virgin olive oil (VOO) polar fraction (PF) before and after acidic hydrolysis of their bound forms. PF extraction and hydrolysis conditions were as previously reported. The chromatographic run lasts ~1/3 of the time needed under high performance liquid chromatography (HPLC) conditions, this was also examined. Eluent consumption for the same piece of information was 6-fold less. Apart from being cost effective, a larger number of samples can be analyzed daily with less environmental impact. Two external curves, detection at 280 nm and correction factors for molecular weight difference are proposed. The method, which is fit for purpose, is selective, robust with satisfactory precision (percentage relative standard deviation (%RSD) values < 11%) and recoveries higher than 87.6% for the target analytes (Htyr, Tyr). Standard operational procedures are easy to apply in the olive oil sector

Toward a harmonized and standardized protocol for the determination of total hydroxytyrosol and tyrosol content in virgin olive oil (VOO). The pros of a fit for the purpose ultra high performance liquid chromatography (UHPLC) procedure

\u3a4oward a harmonized and standardized procedure for the determination of total hydroxytyrosol and tyrosol content in virgin olive oil (VOO), the pros of a recently published in house validated ultra high performance liquid chromatography (UHPLC) protocol are discussed comparatively with those of other procedures that determine directly or indirectly the compounds hosted under the health claim on "olive oil polyphenols" (EC regulation 432/2012). Authentic VOOs were analyzed with five different liquid chromatographic separation protocols and 1H-NMR one in five different laboratories with expertise in VOO phenol analysis within three months. Data comparison indicated differences in absolute values. Method comparison using appropriate tools (Passing-Bablok regression and Bland Altman analyses) for all protocols vs. the UHPLC one indicated slight or statistically significant differences. The results were also discussed in terms of cost effectiveness, detection means, standard requirements and ways to calculate the total hydroxytyrosol and tyrosol content. Findings point out that the in-house validated fit for the purpose UHPLC protocol presents certain pros that should be exploited by the interested parties. These are the simplicity of sample preparation, fast elution time that increase the number of samples analyzed per day and integration of well-resolved peaks with the aid of only two commercially available external standards. Importance of correction factors in the calculations is stressed

Impact of the malaxation temperature on the phenolic profile of cv. Cobrançosa olive oils and assessment of the related health claim

Phenolic compounds contribute to the bioactive properties of olive oil. However, olive oils can only support a health claim concerning the protection against oxidative stress depending on the polyphenolic concentration, requiring effective measures during extraction to preserve/enhance their concentrations. The effect of the malaxation temperature (22, 28 and 34 °C) on the phenolic profile was studied for industrially extracted cv. Cobrançosa oils. Higher malaxation temperatures decreased the contents of the majority of the chromatographically detected compounds (P<0.05, one-way ANOVA), enabling oils differentiation. This decreasing trend was observed for hydroxytyrosol and tyrosol bound forms, determinant for the health claim, which were also negatively affected by temperature, despite revealing that all the industrially extracted oils tested supported the health claim. The observed constant free to bound forms ratio showed that the temperature range tested had a minor effect on bound-forms hydrolysis, being both free and bound forms equally affected by temperature.The authors are grateful to the Foundation for Science andTechnology (FCT, Portugal) forfinancial support by national fundsFCT/MCTES to CIMO (UIDB/00690/2020), to CEB (UIDB/04469/2020), to REQUIMTE-LAQV (UIDB/50006/2020) and to BioTecNorteoperation (NORTE‐01‐0145‐FEDER‐000004) funded by the EuropeanRegional Development Fund under the scope of Norte2020‐Programa Operacional Regional do Norte. Ítala Marx acknowledges the Ph.D.research grant (SFRH/BD/137283/2018) provided by FCT. NunoRodrigues thanks the National funding by FCT- Foundation for Scienceand Technology, P.I., through the institutional scientific employment program-contract.info:eu-repo/semantics/publishedVersio

Impact of phenolic-rich olive leaf extract on blood pressure, plasma lipids and inflammatory markers: a randomised controlled trial

Purpose Dietary polyphenols have been demonstrated to favourably modify a number of cardiovascular risk markers such as blood pressure (BP), endothelial function and plasma lipids. We conducted a randomised, double-blind, controlled, crossover trial to investigate the effects of a phenolic-rich olive leaf extract (OLE) on BP and a number of associated vascular and metabolic measures. Methods A total of 60 pre-hypertensive [systolic blood pressure (SBP): 121–140 mmHg; diastolic blood pressure (DBP): 81–90 mmHg] males [mean age 45 (±SD 12.7 years, BMI 26.7 (±3.21) kg/m2] consumed either OLE (136 mg oleuropein; 6 mg hydroxytyrosol) or a polyphenol-free control daily for 6 weeks before switching to the alternate arm after a 4-week washout. Results Daytime [−3.95 (±SD 11.48) mmHg, p = 0.027] and 24-h SBP [−3.33 (±SD 10.81) mmHg, p = 0.045] and daytime and 24-h DBP [−3.00 (±SD 8.54) mmHg, p = 0.025; −2.42 (±SD 7.61) mmHg, p = 0.039] were all significantly lower following OLE intake, relative to the control. Reductions in plasma total cholesterol [−0.32 (±SD 0.70) mmol/L, p = 0.002], LDL cholesterol [−0.19 (±SD 0.56) mmol/L, p = 0.017] and triglycerides [−0.18 (±SD 0.48), p = 0.008] were also induced by OLE compared to control, whilst a reduction in interleukin-8 [−0.63 (±SD 1.13) pg/ml; p = 0.026] was also detected. Other markers of inflammation, vascular function and glucose metabolism were not affected. Conclusion Our data support previous research, suggesting that OLE intake engenders hypotensive and lipid-lowering effects in vivo

Sobre la determinación de ácidos fenólicos minoritarios de aceite de oliva virgen mediante RP-HPLC

The objective of this study was the detection and determination of four minor phenolic acids present in the polar fraction of olive oil. Gallic, homovanillic, caffeic and ferulic acids, were separated on RP-HPLC and detected by using three different systems. Detection limits were determined for the four compounds. Variable wavelength UV detectors were found to be more suitable than diode array for quantitative information. However, diode array was required for qualitative information for unknown components present in olive oil. For the determination of sensitive phenolic compouds present in minor amounts the use of a more sensitive system, such as the electrochemical detector, was necessary.El objetivo de este estudio fue la detección y determinación de cuatro ácidos fenólicos minoritarios presentes en la fracción polar del aceite de oliva. Los ácidos gálico, homovanílico, cafeico y ferúlico fueron separados mediante RP-HPLC y detectados usando tres sistemas diferentes. Se determinaron los límites de detección para los cuatro componentes. Se encontró que los detectores UV a longitud de onda variable son más apropiados que los detectores de batería de diodos para la información cuantitativa. Sin embargo, el detector de batería de diodo fue necesario para la información cualitativa de componentes desconocidos en el aceite de oliva. Para la determinación de compuestos fenólicos sensibles, presentes en cantidades minoritarias, fue necesario el uso de un sistema más sensible, como es el detector electroquímico