New method for determination of (E)‐resveratrol in wine based on microextraction using packed sorbent and ultra‐performance liquid chromatography

Abstract

An ultra-fast and improved analytical methodology based on microextraction by packed sorbent (MEPS) combined with ultra-performance LC (UPLC) was developed and validated for determination of (E)-resveratrol in wines. Important factors affecting the performance of MEPS such as the type of sorbent material (C2, C8, C18, SIL, and M1), number of extraction cycles, and sample volume were studied. The optimal conditions of MEPS extraction were obtained using C8 sorbent and small sample volumes (50-250 mL) in one extraction cycle (extract-discard) and in a short time period (about 3 min for the entire sample preparation step). (E)-Resveratrol was eluted by 1  250 mL of the mixture containing 95% methanol and 5% water, and the separation was carried out on a highstrength silica HSS T3 analytical column (100 mm  2.1 mm, 1.8 mm particle size) using a binary mobile phase composed of aqueous 0.1% formic acid (eluent A) and methanol (eluent B) in the gradient elution mode (10 min of total analysis). The method was fully validated in terms of linearity, detection (LOD) and quantification (LOQ) limits, extraction yield, accuracy, and inter/intra-day precision, using a Madeira wine sample (ET) spiked with (E)-resveratrol at concentration levels ranging from 5 to 60 mg/mL. Validation experiments revealed very good recovery rate of 9575.8% RSD, good linearity with r 2 values 40.999 within the established concentration range, excellent repeatability (0.52%), and reproducibility (1.67%) values (expressed as RSD), thus demonstrating the robustness and accuracy of the MEPS C8 /UPLC-photodiode array (PDA) method. The LOD of the method was 0.21 mg/mL, whereas the LOQ was 0.68 mg/mL. The validated methodology was applied to 30 commercial wines (24 red wines and six white wines) from different grape varieties, vintages, and regions. On the basis of the analytical validation, the MEPS C8 /UPLC-PDA methodology shows to be an improved, sensitive, and ultra-fast approach for determination of (E)-resveratrol in wines with high resolving power within 6 min.

A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

“…In recent years, the ability of several extraction techniques, such as solid-liquid extraction (SLE) [19], enzyme-assisted extraction [20], heat extraction [21], solid-phase extraction (SPE) [22], and solid-phase microextraction (SPME) [23], for the isolation free low molecular-weight polyphenols (LMW-PPs) from vegetables and other food matrices, has been proposed and evaluated as reliable alternatives to classic liquid-liquid extraction (LLE) technique. More recently, a novel analytical approach, based on miniaturized microextraction by packed sorbent (MEPS), followed by ultrahigh pressure liquid chromatography (UHPLC) separation, has been proposed by Gonç alves et al [24] for quantitative determination of wine biologically active phenolic constituents and trans-resveratrol [25]. In the last few years, a quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique for the multiclass, multiresidue analysis of pesticides in fruits and vegetables, was described by Anastassiades et al [26].…”

Development of a novel microextraction by packed sorbent-based approach followed by ultrahigh pressure liquid chromatography as a powerful technique for quantification phenolic constituents of biological interest in wines

“…Selection of sorbent is an important factor to achieve acceptable clean-up and get high extraction yield [30]. Therefore the performance of the five MEPS sorbent materials: C2 (ethyl-silica), C8 (octyl-silica), C18 (octadecyl-silica), SIL (unmodified silica) and M1 (a mixed mode sorbent containing 80% C8 and 20% strong cationic exchange (SCX)) was tested and compared, in order to select the best sorbent for the target analytes.…”

“…In this context the microextraction by packed sorbent (MEPS) appears as a new format for solid-phase extraction (SPE) that has been miniaturized to work with sample volumes as small as 10 L [29,30]. The commercially available presentation of MEPS uses the same sorbents as conventional SPE columns and so is suitable for use with most existing methods by scaling the reagent and sample volumes.…”

“…Unlike conventional SPE columns, the MEPS sorbent bed is integrated into a liquid handling syringe that allows for low void volume sample manipulations either manually or in combination with laboratory robotics. When the sample has passed through the solid support, the analytes are adsorbed to the solid phase packed in a barrel insert and needle (BIN) [30][31][32] (Fig. 2).…”

Why research on resveratrol-mediated cardioprotection should not decelerate1This editorial was invited by the Editors.

“…The best source of resveratrol in food is considered to be red wine. The average recommended dose of red wine is 2 glasses (approximately 300 mL, which is a conservative estimate), and it has been recently reported that some red wines may contain as much as 40-50 mg resveratrol per litre (Gonçalves and Camara 2011). This would equate to a dose of as much as 15 mg resveratrol in 300 mL of wine, which is slightly lower than that used to improve cardiac structure and function in animal models of ischemic heart disease and hypertension in 2 above-mentioned studies (Chan et al 2011;Lin et al 2008).…”