*2.2. Freeze-Drying Processing*

Oranges were washed, peeled, cut and triturated in a bench top electrical food processor for 40 s at speed 4 (2000 rpm) followed by 40 s at speed 9 (9100 rpm) (Thermomix TM 21, Vorwerk, Spain). The orange puree was mixed for 10 min at speed 3 (1000 rpm) with (5 g GA + 1 g BF)/100 g orange puree as to ensure the physical stability of the dried product [26]. The formulated orange puree (FOP) was distributed in 10.5 × 7.8 cm aluminum plates of 0.5 cm thickness. Samples were immediately frozen at two different freezing rates (FR): slow freezing (FR-S) in a conventional freezer (Liebherr Mediline LGT 2325, Liebherr, Baden-Wurtemberg, Germany) for 48 h and fast freezing (FR-F), where the samples were frozen for 3 h at −38 ◦C in a blast freezer (Hiber RDM051S, Hiber, Cernusco sul Naviglio, Italy), and then stored at −45 ◦C in the conventional freezer for at least 24 h. Frozen samples were dried in a freeze-drier (Telstar Lyoalfa-6, Telstar, Terrassa, Spain) at different pressures (P) in the chamber and shelf temperatures (T). Twelve different conditions were studied (Table 1). The shelf temperature conditioned the drying time, this being 25 h at 30 ◦C, 7 h at 40 ◦C and 6 h at 50 ◦C. The time was selected based on preliminary experiments to be enough to achieve a water content lower than 4%. At these conditions, the physical stability of the formulated puree was known to be guaranteed, as no structural collapse was observed.


**Table 1.** Sample and conditions code according the 12 different freeze-drying conditions studied.

## *2.3. Water Content*

The water content (xw, g water/100 g product) of FOP was determined using the AOAC method [27]. The sample was dried in a vacuum oven (Selecta®, Vaciotem-T, J.P. Selecta S.A., Barcelona, Spain) at 60 ± 1 ◦C under *P* < 100 mm Hg until constant weight (XS204 DeltaRange®, Mettler Toledo, Switzerland). For the freeze-dried puree, an automatic Karl Fisher titrator (Mettler Toledo, Compact Coulometric Titrator C10S, Worthington, OH, USA) was used to obtain the water content. Triplicates were performed in each case.
