Optimisation of a headspace solid-phase microextraction with on-fiber derivatisation method for the direct determination of haloanisoles and halophenols in wine

Pizarro, Consuelo; Pérez-del-Notario, N.; González-Sáiz, J.M.

doi:10.1016/j.chroma.2007.01.023

Cited by 50 publications

(30 citation statements)

References 43 publications

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“…Another parameter that must be taken into consideration is the ionic strength once this greatly influences the partitioning coefficient of the solutes between the liquid and vapour phases. An increment of salt concentration increases the extraction efficiency due to the decrease of analytes solubility, which improves sensitivity by promoting higher enrichment into the stationary phase [31]. Thus, the ionic strength was tested at 0, 10, 20 and 30% of NaCl (w/v) using the DVB/CAR/PDMS fibre (60 min at 25 • C) and the results obtained are depicted in Fig.…”

Section: Hs-spme Optimisationmentioning

confidence: 99%

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

Perestrelo

Nogueira

2009

Talanta

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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.

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Section: Hs-spme Optimisationmentioning

confidence: 99%

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

Perestrelo

Nogueira

2009

Talanta

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“…On the other hand, for specific applications, the choice of a suitable solid-phase, depends on the class of compounds be analyzed, e.g. CAR/PDMS for volatile sulphides and disulphides (Mestres et al, 1999), on-fibre derivatization (PA) for the determination of haloanisoles and halophenols (Pizarro et al, 2007).…”

Section: Sorptive-based Techniquesmentioning

confidence: 99%

Application of Gas Chromatography on the Evaluation of Grape and Wine Aroma in Atlantic Viticulture (NW Iberian Peninsula)

Vilanova¹,

Oliveira²

2012

Gas Chromatography in Plant Science, Wine Technology, Toxicology and Some Specific Applications

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“…For instance, HS-SPME is highly exploited in characterizing wine components (Mestres et al, 1999a,b;Pizarro et al, 2007), trace quantitative analyses of benzene, toluene, ethylbenzene and xylenes (BTEX) in water (Matisová et al, 2002), BTX in blood (Alegretti et al, 2004) and urine (Alkalde et al, 2004) samples, perfluorocarbons in blood (Mathurin et al, 2001), furans (Altaki et al, 2007) and fungicides (Navalón et al, 2002b) found in various food, for the HS-rich, complex matrix of bergamot oil (Tranchida et al, 2006) and especially for chlorinated VOC (Liu et al, 2008;Antoniou et al, 2006), organochlorine pesticides (Aguilar et al, 1999) and methyl tert-butyl ether (MTBE) (Dron et al, 2002) in water. HS-SPME is even used in the artificial fiber industry to detect impurities produced from toluene in industrial caprolactam (Li and Zou, 2006).…”

Section: Introductionmentioning

confidence: 99%

“…higher efficiency) and hence, being timesaving, especially as the number of experimental variables increases (Ferreira et al, 2004(Ferreira et al, , 2007Araujo et al, 2006). Doehlert design has been utilized for optimizing chromatographic/ detector conditions (Tak et al, 2007), determining optimal levels of internal standards for quantification (Araujo et al, 2006) and foremost for optimizing DI-SPME/HS-SPME for analyzing a variety of analytes (Aguilar et al, 1999;Navalón et al, 2002a;Pizarro et al, 2007).…”

Section: Introductionmentioning

confidence: 99%

Optimization of a novel headspace–solid‐phase microextraction–gas chromatographic method by means of a Doehlert uniform shell design for the analysis of trace level ethylene oxide residuals in sterilized medical devices

DiCicco

Láng

Harper

2009

Biomedical Chromatography

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Medical devices sterilized by ethylene oxide (EtO) retain trace quantities of EtO residuals, which may irritate patients' tissue. Reliably quantifying trace level EtO residuals in small medical devices requires an extremely sensitive analytical method. In this research, a Doehlert uniform shell design was utilized in obtaining a response surface to optimize a novel headspace-solid-phase microextraction-gas chromatographic (HS-SPME-GC) method developed for analyzing trace levels of EtO residuals in sterilized medical devices, by evaluating sterilized, polymer-coated, drug-eluting cardiovascular stents. The effects of four independent experimental variables (HS-SPME desorption time, extraction temperature, GC inlet temperature and extraction time) on GC peak area response of EtO were investigated simultaneously and the most influential experimental variables determined were extraction temperature and GC inlet temperature, with the fitted model showing no evidence of lack-of-fit. The optimized HS-SPME-GC method demonstrated overall good linearity/linear range, accuracy, repeatability, reproducibility, absolute recovery and high sensitivity. This novel method was successfully applied to analysis of trace levels of EtO residuals in sterilized/aerated cardiovascular stents of various lengths and internal diameter, where, upon heating, trace EtO residuals fully volatilized into HS for extraction, thereby nullifying matrix effects. As an alternative, this novel HS-SPME-GC method can offer higher sensitivity compared with conventional headspace analyzer-based sampling.

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Optimisation of a headspace solid-phase microextraction with on-fiber derivatisation method for the direct determination of haloanisoles and halophenols in wine

Cited by 50 publications

References 43 publications

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

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

Application of Gas Chromatography on the Evaluation of Grape and Wine Aroma in Atlantic Viticulture (NW Iberian Peninsula)

Optimization of a novel headspace–solid‐phase microextraction–gas chromatographic method by means of a Doehlert uniform shell design for the analysis of trace level ethylene oxide residuals in sterilized medical devices

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