Quantification of oleacein and oleuropein aglycone in olive oil using deuterated surrogates by normal‐phase ultra high performance liquid chromatography with quadrupole time‐of‐flight mass spectrometry

Abstract

An analytical method for the analysis of relevant secoiridoid‐based components in olive oil, oleacein and oleuropein aglycone, is described using for the first time deuterated surrogates. 0.2 g of sample was necessary to perform the analysis using liquid‐liquid extraction and ultrasound‐assisted extraction with a mixture of methanol/water (4:1, v/v). To avoid the formation of by‐products, normal‐phase ultra high performance liquid chromatography was chosen for the chromatographic separation. The selected mobile phase was a gradient mixture of tetrahydrofurane and hexane, and an ACE Excel 3 CN‐ES column as stationary phase. The detection and quantification was performed with a SYNAPT G2‐Si mass spectrometer. The calibration curves for oleacein and oleuropein aglycone were linear and quadratic, respectively. The validation was done at three levels of concentration. Relative errors from 0.1 to 10.5% and relative standard deviations lower than 9% were obtained. The method was applied to study different samples of olive oil.

Extraction, Analysis, and Antioxidant Activity Evaluation of Phenolic Compounds in Different Italian Extra-Virgin Olive Oils

“…Peak area precision, intra-day, and day-to-day resulted in being in the range of 5.9–10.2% and 5.8–10.5%, respectively. RSD% values are acceptable and in accordance to the ones obtained for other published EVOO phenolic compounds analysis methods [32,33]. Linearity was studied analyzing a standard mixture containing 4-hydroxyphenylacetic acid, p-coumaric acid, vanillic acid, oleuropein, apigenin, pinoresinol, luteolin, and 2-(4-hydroxyphenyl)ethanol at concentration range for each analyte of LOQ-140 mg·L −1 without an internal standard.…”

Direct determination of phenolic secoiridoids in olive oil by ultra-high performance liquid chromatography-triple quadruple mass spectrometry analysis

“…Using surrogates is convenient in any analytical method that involves sample extraction. A stable-isotope-labeled (SIL) analogue of the analyte is the most appropriate surrogate in a quantitative analysis by LC-MS and since these are very scarce for phenolic secoiridoids 16 , the method described in this publication is highly recommended. Additionally, LC-MS determination of phenolic secoiridoids with pure standards of all the analytes is the most reliable and accurate situation 55 .…”

“…Several analytical methods have been reported in the last two decades to jointly, individually or even with other phenols analyse these four compounds in olive oil using a large number of analytical techniques 10,16–27 . In recent years, reverse phase liquid chromatography with high and low resolution mass detection has been widely used.…”

“…A selective method is therefore mandatory. Recently, our group has tried to avoid these drawbacks developing a selective method for the determination of 3 and 5 using deuterated surrogates 16 .…”

Preparative isolation and purification of steroidal glycoalkaloid from the ripe berries of Solanum nigrum L. by preparative HPLC–MS and UHPLC–TOF‐MS/MS and its anti‐non‐small cell lung tumors effects in vitro and in vivo

“…Herbal medicines and herbal constituents are the most suitable and safe alternatives to anti‐cancer medicine . Preparative liquid chromatography high‐performance liquid chromatography‐mass spectrometry (Pre‐HPLC‐MS) and UHPLC‐QTOF‐MS/MS provide superior means for the rapid identification and separation of the active ingredients in natural plants . Solanum nigrum is a widely used plant in Chinese folk medicine for the treatment of cancer .…”