Gh. Zgherea/Chem.J. Mold. 2008, 3 (1),52-55The mixtures <strong>of</strong> mobile phase has the same initially composition, with 45% water. In this instance, the2.4-DNPHAA will be eluted before the 2.4-DNPHD. This way is guaranteed the maximum difference between thevalues <strong>of</strong> retention times for the mentioned 2.4-DNPH-ones and a preliminary separation <strong>of</strong> the 2.4-DNPH-ones withthree and four atoms <strong>of</strong> carbon. The synthetic mixture SM Icontains four 2.4-DNPH-ones in the following ratio <strong>of</strong>volume:2.4-DNPHAA: 2.4-DNPHD: 2.4-DNPHA: 2.4-DNPHiBA = 2:1:1:1.The first program <strong>of</strong> binary mobile phase, BGMP I(32 minutes, figure 1), contains four time segments; in figure2 there are the chromatogram <strong>of</strong> synthetic mixture SM I, obtained with BGMP I.According BGMP I,the separation begins with a mobile phase having 45% water; the mixture <strong>of</strong> mobile phasehas a higher polarity. This mixture is hold during the first time segment, g=1 (t=12 minutes), assuring a better resolutionbetween the signal <strong>of</strong> 2.4-DNPHAA (844 s) and the signal <strong>of</strong> 2.4-DNPHD (918 s). The weak polar molecules <strong>of</strong>two 2.4-DNPH-ones are strongly retained on the no polar stationary phase. Therefore, the longitudinal diffusion <strong>of</strong>concentrated zone is lower. Simultaneously, on the stationary phase are strongly retained the 2.4-DNPH-ones providedby acetone and i-buthanal.Figure 2.The chromatogram <strong>of</strong> synthetic mixture abbreviate SM IAA is the chromatographic signal for the 2.4-DNPHAAand 844 is the retention time, in seconds;D represents the chromatographic signal for the2.4-DNPHD and 918 is the retention time (seconds);A represents the chromatographic signal for the2.4-DNPHA and 1280 is the retention time (seconds);iBA represents the chromatographic signal for the2.4-DNPHiBA and 1460 is the retention time (seconds).On the second timing segment, g=2 (t=10 min, n=0.1), the percent <strong>of</strong> water will be reduce at 20%, thus thepolarity <strong>of</strong> mobile phase subside; the 2.4-DNPHAA and 2.4-DNPHD (more soluble in organic solvent) diffuse in themobile phase and will be transported to the end <strong>of</strong> separation column. On the third timing segment, g=3 (t=5 min, n=1),the percent <strong>of</strong> water is constant (20%), to assure the best separation <strong>of</strong> 2.4-DNPHA and 2.4-DNPHiBA. The last timingsegment, g=9 (t=5 min, n=5.5), is destined to recondition stationary phase, for a new separation; all the timing segmentsg=4-8 are inactive.Figure 3. The program <strong>of</strong> GBMP II53
Gh. Zgherea/Chem.J. Mold. 2008, 3 (1),52-55The second program <strong>of</strong> binary mobile phase, BGMP II(40 minutes, figure 3), contains four time segments too;in figure 4 there are the chromatogram <strong>of</strong> synthetic mixture SM II, obtained with BGMP II. The synthetic mixture SM IIcontains the same 2.4DNPH-ones as SM I, in the ratio <strong>of</strong> volume:2.4-DNFHAA: 2.4-DNFHD: 2.4-DNFHA: 2.4-DNFHiBA = 4:1:5:5.As in previous case, the first timing segment, g=1 (t=15 min), the mixing program assures an eluent with 45%water, for the best separation between 2.4-DNPHAA and 2.4-DNPHD; the polarity <strong>of</strong> mobile phase is higher (themolecules <strong>of</strong> 2.4-DNPH-ones are strongly retained on the stationary phase).The second timing segment, g=2 (t=10min, n=9.9), the percent <strong>of</strong> water is reduced at 20%; this value is constantand during the third timing segment, g=3 (t=15min). Subside <strong>of</strong> mobile phase polarity produce a desorbtive processfrom the stationary phase. The timing segments, g=4-8 haven’t got a specific content. In the last timing segment, g=9(t=5min, n=0.1) quickly rebuilds the initial mixture <strong>of</strong> mobile phase; at the finish, the analytical system is completelyready to a new separation.Comparing the chromatograms from figures 2 and 4, may be concluded that the BGMP Iassure a better separationfor the 2.4-DNPHAA and 2.4-DNPHD; for the 2.4-DNPHA and 2.4-DNPHiBA, the resolution is comparable.The figure 5 is a chromatogram <strong>of</strong> a natural mixture <strong>of</strong> 2.4-DNPH-ones, for the inferior carbonyl compounds <strong>of</strong>beer. The liquid-chromatographic separation is on the same column and the eluting program GBMP I.Figure 4.The chromatogram <strong>of</strong> SM IIAA - chromatographic signal for the 2.4-DNPHAA;D - chromatographic signal for the 2.4-DNPHD;A - chromatographic signal for the 2.4-DNPHA(after the same retention time appear the signal forpropanal);iBA - chromatographic signal for the 2.4-DNPHiBA.Figure 5.The chromatogram <strong>of</strong>natural mixture <strong>of</strong> 2.4-DNFH-onesUsing the external standard method, for the chromatographic signal <strong>of</strong> 2.4-DNPHAA, obtain 14.75 mg· L -1 asconcentration <strong>of</strong> acetic aldehyde in beer; the value is in concordance with the literature. The surface <strong>of</strong> chromatographicsignal <strong>of</strong> 2.4-DNPHD <strong>of</strong>fer a value <strong>of</strong> 2.5 mg·L -1 as concentration <strong>of</strong> diacetyl in beer; this value is higher. In beer, thenormal values <strong>of</strong> diacetyl concentration is 0.01-0.2 mg·L -1 ; 0.15 mg·L -1 is the threshold value.ConclusionsOn the basis <strong>of</strong> these experiments may be formulating the following conclusions:1.Was established two optimal programs for providing mixtures <strong>of</strong> binary eluent; according them, it is provided54
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