PMID- 22340891
OWN - NLM
STAT- MEDLINE
DCOM- 20120424
LR  - 20191210
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1230
DP  - 2012 Mar 23
TI  - Automated and quantitative headspace in-tube extraction for the accurate 
      determination of highly volatile compounds from wines and beers.
PG  - 1-7
LID - 10.1016/j.chroma.2012.01.037 [doi]
AB  - An automatic headspace in-tube extraction (ITEX) method for the accurate 
      determination of acetaldehyde, ethyl acetate, diacetyl and other volatile 
      compounds from wine and beer has been developed and validated. Method accuracy is 
      based on the nearly quantitative transference of volatile compounds from the 
      sample to the ITEX trap. For achieving that goal most methodological aspects and 
      parameters have been carefully examined. The vial and sample sizes and the 
      trapping materials were found to be critical due to the pernicious saturation 
      effects of ethanol. Small 2 mL vials containing very small amounts of sample (20 
      muL of 1:10 diluted sample) and a trap filled with 22 mg of Bond Elut ENV resins 
      could guarantee a complete trapping of sample vapors. The complete extraction 
      requires 100 x 0.5 mL pumping strokes at 60  degrees C and takes 24 min. Analytes are 
      further desorbed at 240  degrees C into the GC injector under a 1:5 split ratio. The 
      proportion of analytes finally transferred to the trap ranged from 85 to 99%. The 
      validation of the method showed satisfactory figures of merit. Determination 
      coefficients were better than 0.995 in all cases and good repeatability was also 
      obtained (better than 7% in all cases). Reproducibility was better than 8.3% 
      except for acetaldehyde (13.1%). Detection limits were below the odor detection 
      thresholds of these target compounds in wine and beer and well below the normal 
      ranges of occurrence. Recoveries were not significantly different to 100%, except 
      in the case of acetaldehyde. In such a case it could be determined that the 
      method is not able to break some of the adducts that this compound forms with 
      sulfites. However, such problem was avoided after incubating the sample with 
      glyoxal. The method can constitute a general and reliable alternative for the 
      analysis of very volatile compounds in other difficult matrixes.
CI  - Copyright (c) 2012 Elsevier B.V. All rights reserved.
FAU - Zapata, Julian
AU  - Zapata J
AD  - Laboratory for Flavor Analysis and Enology, Institute of Engineering of Aragon, 
      I3A. Department of Analytical Chemistry, Faculty of Sciences, University of 
      Zaragoza, 50009 Zaragoza, Spain.
FAU - Mateo-Vivaracho, Laura
AU  - Mateo-Vivaracho L
FAU - Lopez, Ricardo
AU  - Lopez R
FAU - Ferreira, Vicente
AU  - Ferreira V
LA  - eng
PT  - Journal Article
PT  - Research Support, Non-U.S. Gov't
PT  - Validation Study
DEP - 20120121
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 0 (Volatile Organic Compounds)
SB  - IM
MH  - Beer/*analysis
MH  - Equipment Design
MH  - Gas Chromatography-Mass Spectrometry/methods
MH  - Limit of Detection
MH  - Sensitivity and Specificity
MH  - Solid Phase Microextraction/*instrumentation
MH  - Volatile Organic Compounds/*analysis
MH  - Wine/*analysis
EDAT- 2012/02/22 06:00
MHDA- 2012/04/25 06:00
CRDT- 2012/02/21 06:00
PHST- 2011/09/05 00:00 [received]
PHST- 2011/11/24 00:00 [revised]
PHST- 2012/01/13 00:00 [accepted]
PHST- 2012/02/21 06:00 [entrez]
PHST- 2012/02/22 06:00 [pubmed]
PHST- 2012/04/25 06:00 [medline]
AID - S0021-9673(12)00134-3 [pii]
AID - 10.1016/j.chroma.2012.01.037 [doi]
PST - ppublish
SO  - J Chromatogr A. 2012 Mar 23;1230:1-7. doi: 10.1016/j.chroma.2012.01.037. Epub 
      2012 Jan 21.