Potentialities of two solventless extraction approaches—Stir bar sorptive extraction and headspace solid-phase microextraction for determination of higher alcohol acetates, isoamyl esters and ethyl esters in wines

Abstract

a b s t r a c tA stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography-quadrupole mass spectrometry (SBSE-LD/LVI-GC-qMS) was evaluated for the simultaneous determination of higher alcohol acetates (HAA), isoamyl esters (IsoE) and ethyl esters (EE) of fatty acids. The method performance was assessed and compared with other solventless technique, the solidphase microextraction (SPME) in headspace mode (HS). For both techniques, influential experimental parameters were optimised to provide sensitive and robust methods. The SBSE-LD/LVI methodology was previously optimised in terms of extraction time, influence of ethanol in the matrix, liquid desorption (LD) conditions and instrumental settings. Higher extraction efficiency was obtained using 60 min of extraction time, 10% ethanol content, n-pentane as desorption solvent, 15 min for the back-extraction period, 10 mL min −1 for the solvent vent flow rate and 10• C for the inlet temperature. For HS-SPME, the fibre coated with 50/30 m divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) afforded highest extraction efficiency, providing the best sensitivity for the target volatiles, particularly when the samples were extracted at 25• C for 60 min under continuous stirring in the presence of sodium chloride (10% (w/v)). Both methodologies showed good linearity over the concentration range tested, with correlation coefficients higher than 0.984 for HS-SPME and 0.982 for SBES-LD approach, for all analytes. A good reproducibility was attained and low detection limits were achieved using both SBSE-LD (0.03-28.96 g L −1 ) and HS-SPME (0.02-20.29 g L −1 ) methodologies. The quantification limits for SBSE-LD approach ranging from 0.11 to 96.56 g L − and from 0.06 to 67.63 g L −1 for HS-SPME. Using the HS-SPME approach an average recovery of about 70% was obtained whilst by using SBSE-LD obtained average recovery were close to 80%. The analytical and procedural advantages and disadvantages of these two methods have been compared.Both analytical methods were used to determine the HAA, IsoE and EE fatty acids content in "Terras Madeirenses" table wines. A total of 16 esters were identified and quantified from the wine extracts by HS-SPME whereas by SBSE-LD technique were found 25 esters which include 2 higher alcohol acetates, 4 isoamyl esters and 19 ethyl esters of fatty acids. Generally SBSE-LD provided higher sensitivity with decreased analysis time.

Comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry combined with solid phase microextraction as a powerful tool for quantification of ethyl carbamate in fortified wines. The case study of Madeira wine

“…The SPME coating fibre and the experimental parameters were adopted from a methodology previously developed in our laboratory for wine analysis [28]. As previous tests indicated the potential of this methodology to detected EC, this methodology was adopted to EC determinations.…”

Classification of Chinese Rice Wine According to Geographic Origin and Wine Age Based on Chemometric Methods and SBSE-TD-GC-MS Analysis of Volatile Compounds

“…Because of the increased quantity of stationary phase utilized, SBSE offers increased sensitivity compared with SPME (Tredoux et al, 2008;Maggi et al, 2008;Hayasaka et al, 2003). This new method has been used for identifying the volatile compounds in Madeira wine (Alves et al, 2005) and "Terras Madeirenses" table wines (Perestrelo et al, 2009). …”

Analysis of E,E-farnesol and squalene in makgeolli using stir bar sorptive extraction coupled with gas chromatography-mass spectrometry

“…SBSE has been widely used in several types of applications, especially in thermal desorption (TD) systems coupled with GC-MS analysis. [18][19][20] Compared with conventional techniques, SBSE has been shown to be an environmental friendly alternative due to its ease of use, high selectivity, high sensitivity and reproducibility, and short time requirement. [21][22][23] The total ion chromatogram of the semi-volatile compounds isolated from makgeolli obtained by the SBSE-TD-GCMS is shown in Fig.…”