Table 2.
Parameters of lyophilization and the properties of selected freeze-dried products.
| Dried Material | Material Size and Form | Freezing Parameters | Shelf Temperature | Pressure of the Chamber | Drying Time | Properties of Material | Ref. |
|---|---|---|---|---|---|---|---|
| Abalone | Cylindrical disks (2.5 cm diameter and 0.7 cm height) | −40 °C | −45, −30, −20, −10, −5, 0, 10, and 15 °C | 100 Pa | 72 h | The increase of a shelf temperature in the range of −45–15 °C caused an increase of the apparent density of dried abalone from 372.9 to 472.1 kg/m3 and a decrease of apparent porosity from 0.733 to 0.664. | [93] |
| Apple | Cylindrical disks (2.5 cm diameter and 0.7 height) | −40 °C | −45, −30, −20, −10, −5, 0, 10, and 15 °C | 100 Pa | 72 h | The increase of a shelf temperature in the range of −45–15 °C caused an increase of apparent porosity from 0.876 to 0.910. | [93] |
| Semi-circular slices (55 mm in length, 2.2–2.5 mm thick) | −25 °C | −25 °C at 1st step drying, 40 °C at 2nd drying |
20 Pa at 1st step drying, 5 Pa at 2nd drying |
24 h | The moisture content was negatively correlated with hardness of freeze-dried apples. The application of freeze-drying resulted in a lower springiness compared to that of the air-drying method. Additionally, the color difference ΔE of freeze-dried apples (11.37) was lower than that obtained for air-dried apples (21.11). | [116] | |
| Puree—layer with thickness of 4 mm | −40 °C | 20 °C | 63 Pa | 26 h | The apple puree freeze-dried at 20 °C absorbed less water than air-dried samples. The application of freeze-drying method enabled the obtainment of powder with a slightly lower hygroscopicity than after microwave-drying. | [130] | |
| Banana | Cylinders with diameter of 20 mm and 8 mm height | −35 °C (48 h), tempered for 1 h in liquid N2 | Product temperature from −50 to −8 °C | 3–300 Pa | 24 h | The values of the bulk density of the banana decreased after freeze-drying from 1900 kg·m−3 to values lower than 400 kg·m−3. The values of bulk density increased (about ~30%) as the temperature of process was increased from −50 to −8 °C. The porosity of freeze-dried banana was the highest at the low temperature of −50 °C (~0.9). | [95] |
| Carrot | Cylinders with diameter of 20 mm and 8 mm height | −35 °C (48 h), tempered for 1 h in liquid N2 | Product temperature from −50 to −5 °C | 3–300 Pa | 24 h | The values of bulk density of carrot tissue decreased after freeze-drying from 1750 kg·m−3 to values lower than 250 kg·m−3. The bulk density values increased (about ~40%) as the temperature of process was increased from −50 to −8 °C. The porosity of freeze-dried carrot was reduced by about 10% after drying at higher temperatures. | [95] |
| Coffee solutions | Layer with thickness of 20 mm | 1 set: −40 °C at 1 °C/min 2 set: fluctuation of temperature between −40 and −20 °C |
−40 °C at the primary drying, 20 °C at the secondary drying |
10 Pa | 18 h | Samples freeze-dried with temperature oscillations (−20 and −40 °C) had larger pores than material frozen at −40 °C. Temperature fluctuations during freezing promoted large crystal formation and resulted in a higher total porosity by, on average, 18%. The application of freezing cycles led to faster reconstruction rates. | [131]: |
| Dragon fruit | Pieces with thickness of 1 cm | −40 °C fast freezing (an air blast freezer and a contact plate freezer) | −5 °C at the primary drying, 30, 40, and 50 °C at the secondary drying |
40 Pa | 50 h at 30 °C, 55 h at 40 °C, 60 h at 50 °C |
The apparent densities of freeze-dried dragon fruits were 0.16, 0.19, and 0.08 g × cm−3 at the drying temperatures 30, 40, and 50 °C, respectively. The hardness of dried fruit decreased from 9.26 to 4.33 N and crispness increased from 6.83 to 10.56 with the increase of the heating temperature. |
[115]: |
| Eggplant | Cubes of 9 mm side | −40 °C | 1 set: −30, −15, and 0 °C at 1st step drying, 20 °C at 2nd step drying 2 set: −30 and 0 °C at 1st drying, 20 °C at 2nd step drying |
1 set: 10 Pa 2 set: 10, 20, and 40 Pa |
1 set: 7–15.3 h 2 set: 14–20.9 h |
The loss of antioxidant capacity was 49.9 and 68.6% for freeze-dried samples dried at −30 and 0 °C, respectively. The increase of drying temperature from −30 to 0 °C caused the loss of ascorbic acid from 37.9 to 12.2%. Total polyphenol content—TPC—in dried product was retained at higher pressures. The loss of TPC was 32.5% at 40 Pa and 47.7% at 10 Pa. | [132]: |
| Garlic | Brick shaped samples (20 × 10 × 10 mm) | −40 °C | −5, −15, and −25 °C | 108 Pa | 72 h | The decrease of shelf temperature from −5 to −25 °C during the freeze-drying of garlic resulted in a decrease of the apparent density from 469 to 431 kg/m3 and an increase of the shrinkage expansion between 0.44 and 0.52, as well as the true density decreased in the range of 1534–1504 kg/m3. | [94]: |
| Grapefruit puree | 1-cm layer | −45 °C | room temperature, 40 °C | 9 Pa | 1.5−21 h | The increase of temperature promoted an increase in the porosity of freeze-dried puree (from 0.78 to 0.83) and a decrease in the number of pores formed from 415to 312. | [16]: |
| Gum Arabic solutions | Layer with a height of 0.5 cm | −40 °C (at 1 °C/min) | −20, −30, and −40 °C at primary during, 20 °C at secondary drying | 10 Pa | 18 h | The degree of puffing was stronger for samples dried at higher (−20 and −30 °C) compared to lower (−40 °C) temperatures of the shelf. The primary drying temperature did not affect the size of pores and pore distribution for solutions with concentrations of 20, 30, 40, and 50%. The mean pore diameter of 60% freeze-dried gum hydrocolloid system increased from 745 to 973 µm with the increase of shelf temperature from −40 to −20 °C. | [88]: |
| Kiwi | Whole fruit (without peel) | −40 °C | n/a | 12, 20, 42, 85, and 103 Pa | n/a | The increase of pressure in the range of 12–100 Pa resulted in a decrease of L* from 65.3 to 58.3, as well as a* values from −2.7 to −6.8, and the increase of b* from 22.3 to 28.3. The higher pressure affected the increase of penetration force for freeze-dried kiwi fruit from 4.3 to 16.2 N. | [121]: |
| Lime juice | Sample juice layer with a thickness from 0.3 to 1.1. cm | −30 °C | −61 °C | 3 Pa | 1–10 h | The freeze-drying of lime juice did not affect acidity (4.10–4.15 g citric ac./100 mL), antioxidant activity (17.5–18.3 mg ascorbic ac./100 mL), and carotenoids content (0.61–0.64 mg ∙100 mL-). Fresh juice and reconstituted freeze-dried juice did not significantly differ in relation to sensory attributes. | [133]: |
| Loco (Concholepas concholepas) (boiled) |
Samples 1 × 1 × 0.5 cm Cubes 0.5 side cm |
−25 °C | n/a | 6,7 Pa and 9.6·10−4 Pa (AFD- atmospheric freeze-drying) |
6.7−12 h | The pore surface of freeze-dried loco obtained at a low pressure was 0.32 m2 pores/m2, while after AFD, this value was half (0.16 pores/m2 material surface). The water absorption capacity of the freeze-dried sample was higher than 1.0 at a low pressure, while at AFD conditions, it was lower than 1.0. | [134]: |
| Maltodextrin sugar–agar solutions | Cube (10 × 10 × 10 mm) samples | −20, −40, and −80 °C, tempered at −80 °C before drying |
Room temperature | 10 Pa | 48 h | The pore size and thickness of pore membranes of the freeze-dried system were reduced with a decrease of the freezing temperature. The system frozen at −80 °C was more resistant to compression than samples frozen at −40 and −20 °C. | [123]: |
| Orange puree | Puree, layer with a thickness of 0.5 mm | −45 °C—slow rate: a conventional freezer −38 °C—fast rate—a blast freezer |
30, 40, and 50 °C | 5 and 100 Pa | 25 h at 30 °C, 7 h at 40 °C, 6 h at 50 °C |
The color attributes L, C*, and h* of freeze-dried orange puree were affected by working pressure. The lower values of L* and higher C* were characteristic for samples dried at the high pressure of 100 Pa. The lower range of h* values between 80.3 and 82.6 was registered for the samples dried at higher pressure (100 Pa) and the temperature of the shelf below 50 °C. The lower pressure of 5 Pa and a higher temperature of 50 °C created more resistant to fracture a freeze-dried sample. The lower degradation of vitamin C was observed for samples dried at 40 and 50 °C than at 30 °C. | [14]: |
| Pepper | Samples and puree with layer of 5 mm | −25 °C | 20, 40, and 60 °C | 63 Pa | 290 min (60 °C) 900 min (20 °C) |
The red pepper freeze-dried at higher temperature 60 °C was characterized by lower values of L* (lightness =35.5), a* (redness =27.6), and b* (yellowness =23.8) than the sample dried at 20 °C (L* = 39.2, a* = 34.8, and b* = 27.0). Additionally, the increase in drying temperature caused a decrease of the total phenolic content (from 12.6 to 11.8 mg GAE/g d.m.) and antioxidant activity (EC50- concentration required to obtain a 50% antioxidant effect) from 21.7 to 26.1 mg d.m./mL). | [11]: |
| Potato | Cylindrical disks (2.5 cm diameter and 0.7 height) | −40 °C | −45, −30, −20, −10, −5, 0, 10, and 15 °C | 100 Pa | 72 h | The increase of a shelf temperature in the range from −45–15 °C caused an increase of apparent density of dried potato from 204.2 to 452.2 kg × m−3 and a decrease of apparent porosity from 0.863 to 0.698. | [93] |
| Rice (cooked) | The layer of 1.8 mm | −18 °C | 90 °C | 80 Pa (initial) and 20 Pa (final) | 12 h | The freeze-dried rice had a better rehydration capacity than the freshly cooked sample. Freeze-drying caused the extensive breakage of the grains. The extent of breakage was dependent on the cooking method and was lower in freeze-dried parboiled rice (3.6–36.9%) than non-parboiled grain (50%). | [118]: |
| n/a | −30 °C for 72 h, tempered for 1 h in liquid N2 | n/a | 4, 13, and 125 Pa | 24 h | The bulk density of freeze-dried rice decreased from ~0.9 to ~0.8 for kernels boiled for 4 min and from ~0.6 to ~0.5 for kernels boiled for longer than 20 min with the decrease of applied pressure from 125 to 4 Pa. The porosity of dried kernels was the highest at low pressures. | [10]: | |
| Strawberry | Whole fruits and slices (5 and 10 mm thick) | −40 °C | 30, 40, 50, 60, and 70 °C | n/a | 12–48 h | The color of strawberries and the volume reduction of fruits did not change in case of different drying temperatures. The percentage of collapsed samples exceeded 20% at drying temperatures higher than 50 °C. | [99]: |
| Yellow dates | Halves | −40 °C | −45, −30, −20, −10, −5, 0, 10, and 15 °C | 100 Pa | 72 h | The increase of a shelf temperature in the range from −45–15 °C caused a decrease of the apparent density of dried dates from 485.1.2 to 205.5 kg·× m−3, as well as an increase of apparent porosity from 0.709 to 0.864. | [93]: |
n/a, not available.