Wine Chemistry and Biochemistry

(Steven Felgate) #1

402 V. Ferreira and J. Cacho


lot of extra and in part, useless effort. In addition, wine extracts obtained following


the total extraction approach are extremely complex with many odors and the olfac-


tometric signals overlap, making very difficult the correct assignment of the identity


of the odorant (Cullere et al. 2004b; Escudero et al. 2004). In spite of all this, most


researchers keep on using these kinds of extracts for the GC-O screening of wine


aromas due to their simplicity and to the existence of some reasonable doubts about


the performance of headspace techniques.


The previous discussion leads to the conclusion that “a priori” headspace tech-


niques should be preferred although, as will be discussed, there are some questions


that as yet do not have a satisfactory answer. Here there are three different alter-


natives: static headspace sampling, dynamic headspace sampling and headspace


solid phase microextraction sampling. Static headspace sampling has been used only


rarely in the GC-O profiling of wines (Guth 1997a) and only as a complementary


technique of a total extraction strategy.Surely this is because a large volume of


headspace has to be injected to obtain clear olfactometric signals, and the presence


of ethanol and water creates serious problems in the chromatography if such a large


volume is injected. In addition, in classicalstatic headspace there is no extract, so


that, the GC-O experiment must be carried out on wine, which could cause problems


arising from the stability and homogeneity of the samples if the experiment is going


to take a long time.


The second possibility is the use of dynamic headspace sampling. This technique


fulfils a priori the requirements for the preparation of extracts for screening by


GC-O. However, the presence of ethanol in the headspaces decreases by factors
as high as two orders of magnitude the capacity of the sorbents most frequently


used for the trapping of volatiles, such as Tenax TA or Porapack Q resins, which


helps to explain why the technique is only seldom used out of our laboratory (Le


Fur et al. 2003). This limitation can be solved by increasing the size of the trap,


by reducing the volume of sample, by using thermal desorption or by using a


most efficient sorbent. The solution given by Le Fur et al. (2003) makes use of


an automated purge and trap unit. Aroma volatiles are purged by a gentle stream


of nitrogen on a small volume of wine and are further trapped in a cartridge filled


with 140 mg of Tenax TA. The volatiles are finally thermally desorbed directly


in the chromatographic column. In this strategy a new aliquot of wine is required


each experiment and the analysis of their results suggests that the technique fails


in transferring to the column some less-volatile but potentially important odorants,


since the last odor detected corresponds toβ-phenylethyl alcohol. Such limitation


could be due to the difficult transference of those compounds from the trap to the


column. The solution given in our laboratory makes use of a type of new generation


sorbents, initially devised for the extraction of polar pesticides from water. These


sorbents have demonstrated to have an amazing ability not only to extract aroma


compounds from wine (Ferreira et al. 2004) but also to trap compounds present in


effluents (Lopez et al. 2003a, 2007). In relation to Tenax TA, these sorbents can


be up to 200 times more efficient, which makes it possible to use a relatively small


amount of sorbent (400 mg) to collect efficiently all the volatiles purged out from
80 mL of wine heated at 37◦C (and diluted with synthetic saliva) by a large stream

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