Air Naturel GOTA Ultrasonic Air Humidifier User Manual Page 49

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IV Congreso Internacional de Ciencia y Tecnología de Alimentos - Córdoba, Argentina 14 a 16 de Noviembre de 2012
39
showed the lowest
h
as well as the lowest . GG-trehalose system had intermediate values. These results
show that the inhibition of trehalose crystallisation was achieved by both gums and especially by VG.
Figure 1: DSC thermograms of freeze dried trehalose systems with 0.1% w/v guar or vinal gums 0.1% (GG
and VG, respectively) or without gums equilibrated in DSC pans at 43 % RH for one day. Arrows show glass
transition (T
g
) and crystallisation and melting enthalpies values are indicated.
Table 1: Degree of total trehalose dihydrate crystallisation () and degree of trehalose dihydrate
crystallisation during humidification (
h
) of freeze dried trehalose systems with 0.1% w/v guar or vinal gums
(GG and VG, respectively) or without gums equilibrated in DSC pans at 43 % RH for one day.
h
trehalose
86.1
74.7
trehalose + GG
64.5
37.1
trehalose + VG
24.3
14.9
Freeze-dried lactose formulations humidified at 33% RH
Lactose samples (with or without gums) equilibrated at 33% HR have a T
g
value around 40°C. Lactose
crystallizes as monohydrate but the crystallisation of the anhydrous form is also possible. In both cases, the
water content of the systems at 33% RH allows lactose crystallisation when the temperature exceeds the T
g
.
Then, isothermal DSC runs were conducted at several temperatures between 50 and 65°C in order to evaluate
lactose crystallisation. As an example of the obtained thermograms, Figure 2 shows those obtained at 55°C.
Earlier and sharper peaks related to lactose crystallisation appeared in lactose-gum termograms. GG-lactose
system showed the earliest and smaller exothermic peak. The VG-lactose system presented a peak at
intermediate times between lactose and GG-lactose systems. The shape of the peak and the crystallisation
enthalpy for the systems containing VG and GG were similar between them. Instead, lactose system without
gum had wider peak of crystallisation for all the temperatures studied. This difference in shape for the
crystallisation peak could be related to a variation of the lactose crystallisation mechanism as a consequence
of the gum presence (Kedward et al, 1998). The same trend was obtained at 60 and 65°C for the three
systems (data not shown) respect to the thermograms showed in Figure 2. At 50°C, only the GG- lactose
system showed crystallisation during 130 minutes-DSC runs.
Figure 3a shows the crystallisation enthalpy as a function of temperature for all studied systems. Lactose
system showed the highest crystallisation enthalpies, which increased for higher temperatures. Both gum-
lactose systems had lower enthalpy values than lactose systems, with similar values between them, which
also remained steady when temperature was increased. The fact that the gum free system presented the
highest crystallisation enthalpy showed that lactose crystallisation thermodynamics is affected in the
presence of both gums.
Fig 3b shows the crystallisation time (the time difference between endset and onset crystallisation, or
induction time). The gum-free system showed the slowest lactose crystallisation rate at all analysed
temperatures. VG and GG systems showed shorter and similar crystallisation times, which decreased slightly
as increasing temperature of the isothermal run at DSC.
25 50 75 100
33.8 J/g
89.6 J/g
15.8 J/g
119.6 J/g
trehalose+ VG
trehalose+ GG
trehalose
2 W/g
crystallization
13.2 J/g
38.0 J/g
melting
Temperature (ºC)
Heat flow (W/g), exo >
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