Method for preparing fruit cell water using freeze-drying technology

Abstract

The invention discloses a method for preparing fruit cell water by freeze drying technology, comprising the following steps: step 1, precooling the freeze dryer, and then putting the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment, the vacuum pulse treatment method is: the first section is 0.8-1KPa, 10s, the second section is 101KPa, 10s, the third section is 0.8-1KPa, 10s, the fourth section is 101KPa, 10s, the fifth section is 200-400Pa, 5min, and the annealing method is: 1-3KPa, the heating plate is heated to 4°C and maintained for 30min. The invention enhances the permeability of plant tissues through vacuum pulses, and then freezes the water in plant cells (mixed with volatile components in plants) into ice through vacuum freezing technology, and combines the annealing process to enlarge the ice crystals in the material, increase the sublimation pore channels, and effectively increase the aroma component content in the cell water.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of fruit cell water, and more specifically, to a method for preparing fruit cell water by utilizing freeze-drying technology. Background Art

[0002] The water in the secretory cells, cavities and ducts, glandular hairs and epidermal cells of plant tissues contains a large amount of flavor components, which stimulate the secretion of the pituitary gland, enzymes and hormones, balance the body's functions, and play a role in beauty and skin care. However, current plant beverages cannot only retain flavor substances and remove sugars, and all of them are added by adding flavors and other ways to give the product flavor. Most of the existing technologies separate the components in plant tissue cells through heat treatment, extrusion, juicing, membrane separation and other technologies. These components include sugar, water, minerals, soluble cellulose, and can also affect the aroma components in the cell water to change the original fragrance of the fruit. Summary of the invention

[0003] An object of the present invention is to solve at least the above problems and to provide at least the advantages which will be described hereinafter.

[0004] Another object of the present invention is to provide a method for preparing fruit cell water using freeze-drying technology, which enhances the permeability of plant tissues through vacuum pulses, and then freezes the water in plant cells (mixed with volatile components in the plants) into ice through vacuum freezing technology. Combined with the annealing process, the ice crystals in the material are enlarged, the sublimation pore channels are increased, and the aroma component content in the cell water is effectively increased.

[0005] In order to achieve these objects and other advantages of the present invention, a method for preparing fruit cell water using freeze-drying technology is provided, comprising the following steps:

[0006] Step 1, pre-cool the freeze dryer, then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment, the vacuum pulse treatment method is: the first section 0.8 ~ 1KPa, 10s, the second section 101KPa, 10s, the third section 0.8 ~ 1KPa, 10s, the fourth section 101KPa, 10s, the fifth section 200 ~ 400Pa, 5min, the annealing method is: 1 ~ 3KPa, the heating plate is heated to 4 ° C, and maintained for 30min;

[0007] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0008] Preferably, in step 1, the freeze dryer is precooled to a cold trap temperature of -40°C.

[0009] Preferably, in step 2, the freezing method is specifically as follows: the vacuum is adjusted to 80-100 Pa, the temperature of the raw material is reduced to -18°C, and the temperature of the heating plate is adjusted to 40-80°C.

[0010] Preferably, in step 2, drying is divided into primary drying and secondary drying, wherein during secondary drying, the temperature of the heating plate is 30 to 50° C., the temperature of the cold trap is -40 to -50° C., and the drying time is 6 to 18 hours.

[0011] Preferably, the primary drying is freeze-dried by indirect heating, and the temperature of the heating plate is set as follows: 75-85°C, 4-6h in the first section; 55-70°C, 4-6h in the second section; 45-50°C, 4-6h in the third section; 30-40°C, 7-10h in the fourth section; 40-50°C, 2-3h in the fifth section.

[0012] Preferably, the cold trap temperature during primary drying is -30 to -50°C.

[0013] Preferably, the fruit cell water is sterilized at 400-600 MPa and 4-20° C. for 10 minutes.

[0014] Preferably, in step 1, before placing the raw material into the freeze dryer, the raw material is pretreated, and the pretreatment method is:

[0015] A1. Cut the raw material into blocks, freeze it with liquid nitrogen, and crush it after freezing to obtain crushed material;

[0016] A2, add medical stone of 0.3 times amount of crushed material into crushed material, put into liquid nitrogen again after mixing and freeze, after freezing, stir to medical stone and crushed material dispersion state under 0 ℃ condition after freezing, carry out step 1 operation again after stirring, namely put into precooled freezer;

[0017] Among them, the medical stone is treated before use, and the treatment method is: first soak the medical stone in a hydrochloric acid solution with a concentration of 7 mol / L for 13 hours, take it out and wash it with water for 3 times for standby; take 10 times the amount of medical stone in a sulfuric acid solution with a concentration of 0.5M, and add 0.1 times the total mass of the medical stone in CH3Si(OH)2CH2CH2CH2N(CH2PO3H)2 to mix to obtain a mixed solution; add the treated medical stone to the mixed solution, place it at 50°C and stir it for 3 hours. After the stirring is completed, take the medical stone out from the mixed solution, and rinse it with clean water three times, and the treatment is completed.

[0018] The present invention has at least the following beneficial effects:

[0019] First, the permeability of plant tissues is enhanced through vacuum pulses, and then the water in plant cells (mixed with volatile components in plants) is frozen into ice through vacuum freezing technology. Combined with the annealing process, the ice crystals in the material are enlarged, increasing the sublimation pore channels. By controlling the vacuum pulse program, vacuum freezing annealing program, freeze-drying process program, condensation melting process, and combining filling and packaging technology, plant cell water with natural flavor ingredients can be obtained, and plant cell water products with flavor ingredients close to the original plants can be produced. Lowering the condensation temperature can increase the types and concentrations of aroma substances. By treating medical stone, the absorption of aroma components by medical stone can be effectively reduced, thereby increasing the content of aroma components in fruit cell water.

[0020] Other advantages, objectives and features of the present invention will be embodied in part through the following description, and in part will be understood by those skilled in the art through study and practice of the present invention. DETAILED DESCRIPTION

[0021] The present invention is further described in detail below in conjunction with embodiments so that those skilled in the art can implement the invention with reference to the description.

[0022] <Example 1>

[0023] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0024] Step 1: pre-cool the freeze dryer, and then put the raw material into the freeze dryer for vacuum pulse treatment. The vacuum pulse treatment method is: 0.8KPa, 10s in the first section, 101KPa, 10s in the second section, 0.8KPa, 10s in the third section, 101KPa, 10s in the fourth section, and 200Pa, 5min in the fifth section. The annealing treatment method is: 1KPa, heating plate is heated to 4°C, and maintained for 30min.

[0025] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0026] The raw material is apple.

[0027] <Example 2>

[0028] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0029] Step 1: pre-cool the freeze dryer, and then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment. The vacuum pulse treatment method is: 0.9 KPa, 10 s in the first section, 101 KPa, 10 s in the second section, 0.9 KPa, 10 s in the third section, 101 KPa, 10 s in the fourth section, and 300 Pa, 5 min in the fifth section. The annealing method is: 2 KPa, heating plate is heated to 4 ° C, and maintained for 30 min;

[0030] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0031] The raw material is strawberry.

[0032] <Example 3>

[0033] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0034] Step 1: pre-cool the freeze dryer, and then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment. The vacuum pulse treatment method is: 1KPa, 10s in the first section, 101KPa, 10s in the second section, 1KPa, 10s in the third section, 101KPa, 10s in the fourth section, and 400Pa, 5min in the fifth section. The annealing method is: 3KPa, heating plate is heated to 4°C and maintained for 30min.

[0035] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0036] The raw material is pear.

[0037] <Example 4>

[0038] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0039] Step 1: pre-cool the freeze dryer, and then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment. The vacuum pulse treatment method is: 0.9 KPa, 10 s in the first section, 101 KPa, 10 s in the second section, 0.9 KPa, 10 s in the third section, 101 KPa, 10 s in the fourth section, and 300 Pa, 5 min in the fifth section. The annealing method is: 2 KPa, heating plate is heated to 4 ° C, and maintained for 30 min;

[0040] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0041] In step 1, the freeze dryer is precooled to a cold trap temperature of -40°C.

[0042] In step 2, the freezing method is specifically as follows: the vacuum is adjusted to 80 Pa, and the temperature of the raw material is reduced to -18°C.

[0043] In step 2, drying is divided into primary drying and secondary drying, wherein the temperature of the heating plate during secondary drying is 30° C., the temperature of the cold trap is −50° C., and the drying is performed for 6 hours.

[0044] The primary drying was performed by indirect heating, and the temperature of the heating plate was set as follows: 7°C, 4 h in the first section; 55°C, 4 h in the second section; 45°C, 4 h in the third section; 30°C, 7 h in the fourth section; and 40°C, 2 h in the fifth section.

[0045] The cold trap temperature during primary drying is -50°C.

[0046] The fruit cell water was sterilized at 400MPa and 4℃ for 10min.

[0047] <Example 5>

[0048] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0049] Step 1: pre-cool the freeze dryer, and then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment. The vacuum pulse treatment method is: 0.9 KPa, 10 s in the first section, 101 KPa, 10 s in the second section, 0.9 KPa, 10 s in the third section, 101 KPa, 10 s in the fourth section, and 300 Pa, 5 min in the fifth section. The annealing method is: 2 KPa, heating plate is heated to 4 ° C, and maintained for 30 min;

[0050] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0051] In step 1, the freeze dryer is precooled to a cold trap temperature of -40°C.

[0052] In step 2, the freezing method is specifically as follows: the vacuum is adjusted to 90 Pa, and the temperature of the raw material is reduced to -18°C.

[0053] In step 2, drying is divided into primary drying and secondary drying, wherein the temperature of the heating plate during secondary drying is 40° C., the temperature of the cold trap is −45° C., and the drying is performed for 12 hours.

[0054] The primary drying adopts indirect heating method for freeze drying, and the temperature of the heating plate is set as follows: 80°C, 5h in the first section; 64°C, 5h in the second section; 47°C, 5h in the third section; 35°C, 8h in the fourth section; and 45°C, 2.5h in the fifth section.

[0055] The cold trap temperature during primary drying is -40°C.

[0056] The fruit cell water was sterilized at 500MPa and 14℃ for 10min.

[0057] <Example 6>

[0058] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0059] Step 1: pre-cool the freeze dryer, and then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment. The vacuum pulse treatment method is: 0.9 KPa, 10 s in the first section, 101 KPa, 10 s in the second section, 0.9 KPa, 10 s in the third section, 101 KPa, 10 s in the fourth section, and 300 Pa, 5 min in the fifth section. The annealing method is: 2 KPa, heating plate is heated to 4 ° C, and maintained for 30 min;

[0060] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0061] In step 1, the freeze dryer is precooled to a cold trap temperature of -40°C.

[0062] In step 2, the freezing method is specifically as follows: the vacuum is adjusted to 100 Pa, and the temperature of the raw material is reduced to -18°C.

[0063] In step 2, drying is divided into primary drying and secondary drying, wherein the temperature of the heating plate during secondary drying is 50° C., the temperature of the cold trap is −40° C., and the drying is performed for 18 hours.

[0064] The primary drying adopts indirect heating method for freeze drying, and the temperature of the heating plate is set as follows: 75-85°C, 4-6h in the first section; 70°C, 6h in the second section; 50°C, 6h in the third section; 40°C, 10h in the fourth section; and 50°C, 3h in the fifth section.

[0065] The cold trap temperature during primary drying is -30°C.

[0066] The fruit cell water was sterilized at 600MPa and 20℃ for 10min.

[0067] <Example 7>

[0068] The method for preparing fruit cell water by freeze-drying technology comprises the following steps:

[0069] Step 1, pre-cool the freeze dryer, then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment, the vacuum pulse treatment method is: the first section 0.8 ~ 1KPa, 10s, the second section 101KPa, 10s, the third section 0.8 ~ 1KPa, 10s, the fourth section 101KPa, 10s, the fifth section 200 ~ 400Pa, 5min, the annealing method is: 1 ~ 3KPa, the heating plate is heated to 4 ° C, and maintained for 30min;

[0070] Step 2: The raw materials after annealing are sequentially frozen and dried, and condensed water is collected to obtain fruit cell water.

[0071] In step 1, the freeze dryer is precooled to a cold trap temperature of -40°C.

[0072] In step 2, the freezing method is specifically as follows: the vacuum is adjusted to 90 Pa, and the temperature of the raw material is reduced to -18°C.

[0073] In step 2, drying is divided into primary drying and secondary drying, wherein the temperature of the heating plate during secondary drying is 40° C., the temperature of the cold trap is −45° C., and the drying is performed for 12 hours.

[0074] The primary drying adopts indirect heating method for freeze drying, and the temperature of the heating plate is set as follows: 80°C, 5h in the first section; 64°C, 5h in the second section; 47°C, 5h in the third section; 35°C, 8h in the fourth section; and 45°C, 2.5h in the fifth section.

[0075] The cold trap temperature during primary drying is -40°C.

[0076] The fruit cell water was sterilized at 500MPa and 14℃ for 10min.

[0077] In step 1, before placing the raw material into the freeze dryer, the raw material is pretreated. The pretreatment method is:

[0078] A1. Cut the raw material into blocks, freeze it with liquid nitrogen, and crush it after freezing to obtain crushed material;

[0079] A2, add medical stone of 0.3 times amount of crushed material into crushed material, put into liquid nitrogen again after mixing and freeze, after freezing, stir to medical stone and crushed material dispersion state under 0 ℃ condition after freezing, carry out step 1 operation again after stirring, namely put into precooled freezer;

[0080] Among them, the medical stone is treated before use, and the treatment method is: first soak the medical stone in a hydrochloric acid solution with a concentration of 7 mol / L for 13 hours, take it out and wash it with water for 3 times for standby; take 10 times the amount of medical stone in a sulfuric acid solution with a concentration of 0.5M, and add 0.1 times the total mass of the medical stone in CH3Si(OH)2CH2CH2CH2N(CH2PO3H)2 to mix to obtain a mixed solution; add the treated medical stone to the mixed solution, place it at 50°C and stir it for 3 hours. After the stirring is completed, take the medical stone out from the mixed solution, and rinse it with clean water three times, and the treatment is completed.

[0081] <Comparative Example 1>

[0082] Fruit cell water was prepared by the method of Example 5, except that vacuum pulse treatment, annealing treatment and vacuum freezing were not used, and the raw materials were only subjected to -40°C air cooling before freeze-drying, that is, the raw materials were placed at -40°C for drying, and condensed water was collected to obtain fruit cell water.

[0083] <Comparative Example 2>

[0084] The fruit cell water was prepared by the method of Example 5, wherein the difference was that the primary drying was at 20° C. for 12 h, and the secondary drying was at 20° C. for 12 h.

[0085] <Comparative Example 3>

[0086] The fruit cell water was prepared by the method of Example 5, wherein the difference was that the primary drying was at 70° C. for 12 h, and the secondary drying was at 70° C. for 12 h.

[0087] <Comparative Example 4>

[0088] Fruit cell water was prepared by the method of Example 7, wherein the differences were as follows: A1, the raw material was cut into blocks, then frozen with liquid nitrogen, and crushed after freezing to obtain a crushed material; A2, 0.3 times the amount of medical stone of the crushed material was added to the crushed material, the mixture was placed in liquid nitrogen for freezing after freezing, and after freezing, the medical stone and the crushed material were stirred at 0°C until the medical stone and the crushed material were dispersed, and after stirring, the operation of step 1 was performed, i.e., the material was placed in a pre-cooled freezer, i.e., the medical stone was not treated and was directly mixed with the crushed material.

[0089] <Experimental Characterization>

[0090] Cell water was prepared by the methods of Example 5, Example 7, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4, wherein peach cell water and Fuji apple cell water were prepared respectively by the method of Example 5, peach cell water was prepared by the method of Example 7, peach cell water was prepared by the method of Comparative Example 1, peach cell water was prepared by the method of Comparative Example 2, peach cell water was prepared by the method of Comparative Example 3, and peach cell water was prepared by the method of Comparative Example 4, and the components in the cell water are shown in Tables 1-7;

[0091] Table 1 Gas chromatography-mass spectrometry data of aroma components in peach cell water prepared in Example 5

[0092]

[0093]

[0094] Table 2 Gas chromatography-mass spectrometry data of aroma components in Fuji apple cell water prepared in Example 5

[0095]

[0096]

[0097]

[0098] Table 3 Gas chromatography-mass spectrometry data of aroma components in peach cell water prepared in Comparative Example 1

[0099]

[0100] Table 4 Gas chromatography-mass spectrometry data of aroma components in peach cell water prepared in comparative example 2

[0101]

[0102]

[0103] Table 5. Gas chromatography-mass spectrometry data of aroma components in peach cell water prepared in Comparative Example 3

[0104]

[0105] Table 6 Gas chromatography-mass spectrometry data of aroma components in peach cell water prepared in Example 7

[0106]

[0107] Note: Compared with Table 1, this table only counts the top ten aroma components.

[0108] Table 7 Gas chromatography-mass spectrometry data of aroma components in peach cell water prepared in comparative example 4

[0109]

[0110] Note: Compared with Table 1, this table only counts the top ten aroma components.

[0111] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the embodiments shown and described herein.

Claims

1. A method for preparing fruit cell water using freeze-drying technology, characterized in that: The following steps are involved: Step 1, pre-cool the freeze dryer, then put the raw material into the freeze dryer for vacuum pulse treatment and annealing treatment, the vacuum pulse treatment method is: the first section 0.8 ~ 1KPa, 10s, the second section 101KPa, 10s, the third section 0.8 ~ 1KPa, 10s, the fourth section 101KPa, 10s, the fifth section 200 ~ 400Pa, 5min, the annealing method is: 1 ~ 3KPa, the heating plate is heated to 4 ° C, and maintained for 30min; Step 2: freezing and drying the raw materials after annealing treatment in sequence, collecting condensed water to obtain fruit cell water; In step 1, before placing the raw material into the freeze dryer, the raw material is pretreated. The pretreatment method is: A1. Cut the raw material into blocks, freeze it with liquid nitrogen, and crush it after freezing to obtain crushed material; A2, add medical stone of 0.3 times amount of crushed material into crushed material, put into liquid nitrogen again after mixing and freeze, after freezing, stir to medical stone and crushed material dispersion state under 0 ℃ condition after freezing, carry out step 1 operation again after stirring, namely put into precooled freezer; Among them, the medical stone is treated before use, and the treatment method is: first soak the medical stone in a hydrochloric acid solution with a concentration of 7 mol / L for 13 hours, take it out and wash it with water for 3 times for standby; take 10 times the amount of medical stone in a sulfuric acid solution with a concentration of 0.5M, and add 0.1 times the total mass of the medical stone in CH3Si(OH)2CH2CH2CH2N(CH2PO3H)2 to mix to obtain a mixed solution; add the treated medical stone to the mixed solution, place it at 50°C and stir it for 3 hours. After the stirring is completed, take the medical stone out from the mixed solution, and rinse it with clean water three times, and the treatment is completed.

2. The method for preparing fruit cell water using freeze-drying technology as claimed in claim 1, characterized in that: In step 1, the freeze dryer is precooled to a cold trap temperature of -40°C.

3. The method for preparing fruit cell water using freeze-drying technology as claimed in claim 1, characterized in that: In step 2, the freezing method is specifically as follows: the vacuum is adjusted to 80-100 Pa, and the temperature of the raw material is reduced to -18°C.

4. The method for preparing fruit cell water using freeze-drying technology as claimed in claim 1, characterized in that: In step 2, drying is divided into primary drying and secondary drying, wherein during secondary drying, the temperature of the heating plate is 30 to 50° C., the temperature of the cold trap is -40 to -50° C., and the drying time is 6 to 18 hours.

5. The method for preparing fruit cell water using freeze-drying technology as claimed in claim 4, characterized in that: The primary drying adopts indirect heating method for freeze drying, and the temperature of the heating plate is set as follows: 75-85°C, 4-6h in the first section; 55-70°C, 4-6h in the second section; 45-50°C, 4-6h in the third section; 30-40°C, 7-10h in the fourth section; 40-50°C, 2-3h in the fifth section.

6. The method for preparing fruit cell water using freeze-drying technology as claimed in claim 5, characterized in that: The cold trap temperature during primary drying is -30 to -50°C.

7. The method for preparing fruit cell water using freeze-drying technology as claimed in claim 4, characterized in that: Sterilize the fruit cell water at 400-600MPa and 4-20℃ for 10 minutes.

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