1. A process for extracting freeze-dried cell sap of rosa damascena is characterized by comprising the following steps: comprises the following steps of (a) carrying out,

s1: adding biological enzyme into the rose flowers, stirring uniformly and crushing the rose flowers;

s2: quickly freezing the rose flowers processed in the step S1 at-45 ℃ to-50 ℃, and heating a material partition plate of a low-temperature vacuum extraction bin to 40-42 ℃; transferring the quick-frozen rose flowers to the material partition plate;

s3: controlling the pressure in the low-temperature vacuum extraction bin to be-0.09 to-0.095 Mpa, and controlling the temperature of a condensation distributor in the low-temperature vacuum extraction bin to be-45 ℃ to-50 ℃ and keeping the temperature; then heating the temperature of the condensation distributor to 45 +/-2 ℃ until ice crystals of the cell stock solution of the condensation distributor are completely melted, and collecting the cell stock solution;

s4: quickly freezing the cell stock solution collected in the step S3 below-18 ℃ until the cell stock solution is completely solidified, and then transferring to room temperature for melting;

s5: filtering the cell stock solution melted in the step S4 by using a microporous filter membrane;

s6: and (4) standing and refrigerating the cell stock solution filtered in the step S5, carrying out alcoholization, and filtering with filter cloth to obtain a finished product of the rose freeze-dried cell sap.

2. The extraction process of lyophilized cell sap of rosa damascena according to claim 1, wherein: the biological enzymes include cellulase and pectinase.

3. The extraction process of lyophilized cell sap of rosa damascena according to claim 1, wherein: the aperture of the microporous filter membrane is 0.22 um.

4. The extraction process of lyophilized cell sap of rosa damascena according to claim 1, wherein: in step S6, the alcoholization time is 60 days, and the aperture of the filter cloth is 300-400 mesh.

5. The extraction process of lyophilized cell sap of rosa damascena according to claim 1, wherein: in the step S6, the refrigeration temperature is 2-8 ℃.

6. The extraction process of lyophilized cell sap of rosa damascena according to claim 1, wherein: the adding amount of the biological enzyme is five per thousand of the weight of the rose flower.

7. A Rosa damascena cell sap, which is characterized by being prepared by the extraction process of the Rosa damascena freeze-dried cell sap as claimed in claim 1.

Background

The rose cell sap is the liquid in rose cells, and is widely applied to cosmetics. At present, the rose cell sap is mainly obtained by distillation, dry distillation, vacuum extraction and other modes.

Patent CN109593610A discloses a method for extracting essential oil from damascene rose, which comprises freezing to break wall, distilling, condensing, and separating oil from water to obtain rose essential oil, wherein in extracting rose essential oil, water is added into rose petal, and then heated and distilled to obtain mixture of cell sap and water, and then separation operation is needed, the extraction rate of rose cell sap is low, and the obtained rose cell sap contains other impurities.

Patent CN111721073A discloses a process for vacuum freeze drying rose flower, wherein rose flower is frozen, dried at elevated temperature, and the gas during drying is collected and condensed at low temperature to obtain rose hydrosol.

Disclosure of Invention

The invention aims to provide an extraction process of freeze-dried rose pith cell sap, which is used for freezing and melting rose flowers and cell sap for multiple times, so that the cell walls of roses are fully broken, rose cell sap is fully collected, and the collection efficiency of the cell sap is improved.

The invention is realized by the following technical scheme:

firstly, quick-freezing the rose flowers at a temperature of between 45 ℃ below zero and 50 ℃ below zero, condensing cell sap into ice, trapping essential oil and aromatic substances, residual active ingredients and natural nutrients in the rose flowers in cells of the rose flowers, then heating the rose flowers under vacuum to gasify the cell sap,

an extraction process of freeze-dried cell sap of Rosa damascena comprises the following steps,

s1: adding biological enzyme into the rose flowers, stirring uniformly and crushing the rose flowers;

s2: quickly freezing the rose flowers processed in the step S1 at-45 ℃ to-50 ℃, and simultaneously heating a material partition plate of a low-temperature vacuum extraction bin to 40-42 ℃; transferring the quick-frozen rose flowers to the material partition plate;

s3: controlling the pressure in the low-temperature vacuum extraction bin to be-0.09 to-0.095 Mpa, controlling the temperature of a condensation distributor in the low-temperature vacuum extraction bin to be-45 to-50 ℃, and keeping the temperature until the rose flowers are dried; then heating the temperature of the condensation distributor to 45 +/-2 ℃ until ice crystals of the cell stock solution of the condensation distributor are completely melted, and collecting the cell stock solution;

s4: quickly freezing the cell stock solution collected in the step S3 below-18 ℃ until the cell stock solution is completely solidified, and then transferring to room temperature for melting;

s5: filtering the cell stock solution melted in the step S4 by using a microporous filter membrane;

s6: and (4) standing and refrigerating the cell stock solution filtered in the step S5, carrying out alcoholization, and filtering with filter cloth to obtain a finished product of the rose freeze-dried cell sap.

Further, the biological enzymes include cellulase and pectinase.

Further, the adding amount of the biological enzyme is five per thousand of the weight of the rose flowers.

Further, the aperture of the microporous filter membrane is 0.22um

Further, in the step S6, the alcoholization time is 60 days, and the aperture of the filter cloth is 300-400 mesh.

Further, in the step S6, the refrigeration temperature is 2 to 8 ℃.

The invention also provides a Damascus rose cell sap prepared by the extraction process.

The invention has at least the following advantages and beneficial effects:

1. the extraction process of the invention comprises the steps of mixing the rose flowers with the biological enzyme, carrying out biological catalysis on the rose flowers under the action of the biological enzyme, accelerating the release of aromatic rose molecules, and breaking the rose flowers to release the juice and the cell sap of the rose flowers, thereby improving the collection efficiency of the cell sap.

2. In the invention, the rose flower and the cell stock solution are frozen and thawed for a plurality of times, the first freezing and thawing realizes partial rupture of the membrane structure of the rose, on one hand, the hydrophobic bond structure of the cell membrane can be ruptured, thereby increasing the hydrophilic performance of the cell, on the other hand, the liquid in the cell is crystallized to form ice crystal grains, so that the cell is expanded and ruptured; the second freezing-thawing causes most of cell wall thalli to be broken, the third freezing-thawing causes the cell structure to be completely broken, and the cell sap in the rose cells can be sufficiently separated from the rose flowers through 3 times of freezing-thawing, so that the collection efficiency of the cell sap is improved.

3. In the invention, the extraction of the cell sap and the drying of the roses are carried out simultaneously, so that not only can pure cell sap be obtained, but also the dried rose pollen can be obtained, and the utilization rate of the roses is improved.

4. In the invention, in the process of extracting the rose cell sap, water is not additionally added, the obtained cell sap is pure and has rich fragrance, the effective extraction rate of the cell sap can reach more than 95%, and the time for drying the rose can be accelerated by 8-10h compared with the direct freezing process at the freeze drying rate.

Detailed Description

Example 1:

the embodiment provides an extraction process of a freeze-dried cell sap of rosa damascena, which comprises the following specific steps;

s1 selecting fresh Rosa damascena flowers, picking for no more than 4h, and cleaning the picked Rosa damascena flowers to obtain clean Rosa damascena flowers; standing clean rose flowers in stainless steel stirring equipment, adding five thousandths of biological enzyme A and biological enzyme B respectively, and stirring for 5min to be uniform; standing the uniformly stirred flowers in stainless steel coarse crushing equipment, and coarsely crushing the flowers into flower fragments less than or equal to 5 mm;

s2, placing the crushed rose into an extraction tray according to the height of 2cm, transferring into a quick-freezing warehouse, controlling the temperature of the quick-freezing warehouse to be-45 ℃, and quickly freezing for 2 h. Heating a material partition plate in the low-temperature vacuum extraction bin to 40 ℃ while quickly freezing, and placing the quickly-frozen rose flowers on the material partition plate;

s3, controlling the pressure in the low-temperature vacuum extraction bin between-0.09 MPa and-0.095 MPa, controlling the temperature of the condensation distributor at-50 ℃, and keeping the condition for 12h, in the low-temperature vacuum condensation bin, continuously gasifying the cell sap in the rose flowers on the material partition plate, volatilizing the aromatic rose molecules into air, condensing the aromatic rose molecules into ice crystals when the aromatic rose molecules are attached to the condensation distributor, almost completely gasifying and solidifying the cell sap in the rose flowers on the condensation distributor after 12h of extraction, and drying the rose flowers. Heating the condensation distributor to 45 ℃ after extraction, circulating for 2h until the aromatic molecule ice crystals in the bin are completely melted, and collecting the rose cell stock solution;

s4 placing the rose cell stock solution in a freezer at-18 deg.C, standing, quickly freezing for 48h, thawing at room temperature, mixing with 10 ton stainless steel storage tank,

s5 and filtering by using a 0.22um microporous filter membrane;

s6, placing the filtered rose cell stock solution in a refrigerator at 2-8 ℃ and standing for alcoholization at low temperature for 60 days, and filtering with 400-mesh filter cloth after alcoholization to obtain the finished product of the Damascus rose cell solution.

Example 2:

the embodiment provides an extraction process of a freeze-dried cell sap of rosa damascena, which comprises the following specific steps;

s1 selecting fresh Rosa damascena flowers, picking for no more than 4h, and cleaning the picked Rosa damascena flowers to obtain clean Rosa damascena flowers; standing clean rose flowers in stainless steel stirring equipment, adding five thousandths of biological enzyme A and biological enzyme B respectively, and stirring for 5min to be uniform; standing the uniformly stirred flowers in stainless steel coarse crushing equipment, and coarsely crushing the flowers into flower fragments less than or equal to 5 mm;

s2, placing the crushed rose into an extraction tray according to the height of 2cm, transferring into a quick-freezing warehouse, controlling the temperature of the quick-freezing warehouse to be-50 ℃, and quickly freezing for 2 h. Heating a material partition plate in the low-temperature vacuum extraction bin to 42 ℃ while quickly freezing, and placing the quickly-frozen rose flowers on the material partition plate;

s3, controlling the pressure in the low-temperature vacuum extraction bin between-0.09 MPa and-0.095 MPa, controlling the temperature of the condensation distributor at-60 ℃, keeping the condition for 12h, continuously gasifying the cell sap in the rose flowers on the material partition plate in the low-temperature vacuum condensation bin, volatilizing the aromatic rose molecules into the air, condensing the aromatic rose molecules into ice crystals when the aromatic rose molecules are attached to the condensation distributor, almost completely gasifying and solidifying the cell sap in the rose flowers on the condensation distributor after 12h of extraction, and drying the rose flowers. Heating the condensation distributor to 50 ℃ after extraction, circulating for 2h until the aromatic molecule ice crystals in the bin are completely melted, and collecting the rose cell stock solution;

s4 placing the rose cell stock solution in a freezer at-18 deg.C, standing, quickly freezing for 48h, thawing at room temperature, mixing with 10 ton stainless steel storage tank,

s5 and filtering by using a 0.22um microporous filter membrane;

s6, placing the filtered rose cell stock solution in a refrigerator at 8 ℃ and standing at low temperature for 60 days for alcoholization, and filtering with 800-mesh filter cloth after alcoholization to obtain the finished product of the Damascus rose cell solution.

Example 3:

the embodiment provides an extraction process of a freeze-dried cell sap of rosa damascena, which comprises the following specific steps;

s1 selecting fresh Rosa damascena flowers, picking for no more than 4h, and cleaning the picked Rosa damascena flowers to obtain clean Rosa damascena flowers; standing clean rose flowers in stainless steel stirring equipment, adding five thousandths of biological enzyme A and biological enzyme B respectively, and stirring for 5min to be uniform; standing the uniformly stirred flowers in stainless steel coarse crushing equipment, and coarsely crushing the flowers into flower fragments less than or equal to 5 mm;

s2, placing the crushed rose into an extraction tray according to the height of 2cm, transferring into a quick-freezing warehouse, controlling the temperature of the quick-freezing warehouse at-48 ℃, and quickly freezing for 2 h. Heating a material partition plate in the low-temperature vacuum extraction bin to 42 ℃ while quickly freezing, and placing the quickly-frozen rose flowers on the material partition plate;

s3, controlling the pressure in the low-temperature vacuum extraction bin between-0.09 MPa and-0.095 MPa, controlling the temperature of the condensation distributor at-55 ℃, keeping the condition for 12h, continuously gasifying the cell sap in the rose flowers on the material partition plate in the low-temperature vacuum condensation bin, volatilizing the aromatic rose molecules into the air, condensing the aromatic rose molecules into ice crystals when the aromatic rose molecules are attached to the condensation distributor, almost completely gasifying and solidifying the cell sap in the rose flowers on the condensation distributor after 12h of extraction, and drying the rose flowers. Heating the condensation distributor to 60 ℃ after extraction, circulating for 2h until the aromatic molecule ice crystals in the bin are completely melted, and collecting the rose cell stock solution;

s4 placing the rose cell stock solution in a freezer at-18 deg.C, standing, quickly freezing for 48h, thawing at room temperature, mixing with 10 ton stainless steel storage tank,

s5 and filtering by using a 0.22um microporous filter membrane;

s6, placing the filtered rose cell stock solution in a refrigerator at 2-8 ℃ and standing for alcoholization at low temperature for 60 days, and filtering with 600-mesh filter cloth after alcoholization to obtain the finished product of the Damascus rose cell solution.

Example 4:

the embodiment provides an extraction process of a freeze-dried cell sap of rosa damascena, which comprises the following specific steps;

s1 selecting fresh Rosa damascena flowers, picking for no more than 4h, and cleaning the picked Rosa damascena flowers to obtain clean Rosa damascena flowers; standing clean rose flowers in stainless steel stirring equipment, adding five thousandths of biological enzyme A and biological enzyme B respectively, and stirring for 5min to be uniform; standing the uniformly stirred flowers in stainless steel coarse crushing equipment, and coarsely crushing the flowers into flower fragments less than or equal to 5 mm;

s2, placing the crushed rose into an extraction tray according to the height of 2cm, transferring into a quick-freezing warehouse, controlling the temperature of the quick-freezing warehouse to be-50 ℃, and quickly freezing for 2 h. Heating a material partition plate in the low-temperature vacuum extraction bin to 40 ℃ while quickly freezing, and placing the quickly-frozen rose flowers on the material partition plate;

s3, controlling the pressure in the low-temperature vacuum extraction bin between-0.09 MPa and-0.095 MPa, controlling the temperature of the condensation distributor at-70 ℃, keeping the condition for 12h, continuously gasifying the cell sap in the rose flowers on the material partition plate in the low-temperature vacuum condensation bin, volatilizing the aromatic rose molecules into the air, condensing the aromatic rose molecules into ice crystals when the aromatic rose molecules are attached to the condensation distributor, almost completely gasifying and solidifying the cell sap in the rose flowers on the condensation distributor after 12h of extraction, and drying the rose flowers. Heating the condensation distributor to 50 ℃ after extraction, circulating for 2h until the aromatic molecule ice crystals in the bin are completely melted, and collecting the rose cell stock solution;

s4 placing the rose cell stock solution in a freezer at-18 deg.C, standing, quickly freezing for 48h, thawing at room temperature, mixing with 10 ton stainless steel storage tank,

s5 and filtering by using a 0.22um microporous filter membrane;

s6, placing the filtered rose cell stock solution in a refrigerator at 2-8 ℃ and standing for alcoholization at low temperature for 60 days, and filtering with 600-mesh filter cloth after alcoholization to obtain the finished product of the Damascus rose cell solution.

Example 5

The embodiment provides an extraction process of a freeze-dried cell sap of rosa damascena, which comprises the following specific steps;

s1 selecting fresh Rosa damascena flowers, picking for no more than 4h, and cleaning the picked Rosa damascena flowers to obtain clean Rosa damascena flowers; standing clean rose flowers in stainless steel stirring equipment, adding five thousandths of biological enzyme A and biological enzyme B respectively, and stirring for 5min to be uniform; standing the uniformly stirred flowers in stainless steel coarse crushing equipment, and coarsely crushing the flowers into flower fragments less than or equal to 5 mm;

s2, placing the crushed rose into an extraction tray according to the height of 2cm, transferring into a quick-freezing warehouse, controlling the temperature of the quick-freezing warehouse at-45 ℃, and quickly freezing for 2 h. Heating a material partition plate in the low-temperature vacuum extraction bin to 42 ℃ while quickly freezing, and placing the quickly-frozen rose flowers on the material partition plate;

s3, controlling the pressure in the low-temperature vacuum extraction bin between-0.09 MPa and-0.095 MPa, controlling the temperature of the condensation distributor at-50 ℃, and keeping the condition for 12h, in the low-temperature vacuum condensation bin, continuously gasifying the cell sap in the rose flowers on the material partition plate, volatilizing the aromatic rose molecules into air, condensing the aromatic rose molecules into ice crystals when the aromatic rose molecules are attached to the condensation distributor, almost completely gasifying and solidifying the cell sap in the rose flowers on the condensation distributor after 12h of extraction, and drying the rose flowers. Heating the condensation distributor to 45 ℃ after extraction, circulating for 2h until the aromatic molecule ice crystals in the bin are completely melted, and collecting the rose cell stock solution;

s4 placing the rose cell stock solution in a freezer at-18 deg.C, standing, quickly freezing for 48h, thawing at room temperature, mixing with 10 ton stainless steel storage tank,

s5 and filtering by using a 0.22um microporous filter membrane;

s6, placing the filtered rose cell stock solution in a refrigerator at 2-8 ℃ and standing for alcoholization at low temperature for 60 days, and filtering with 700-mesh filter cloth after alcoholization to obtain the finished product of the Damascus rose cell solution.

Example 6

The embodiment provides an extraction process of a freeze-dried cell sap of rosa damascena, which comprises the following specific steps;

s1 selecting fresh Rosa damascena flowers, picking for no more than 4h, and cleaning the picked Rosa damascena flowers to obtain clean Rosa damascena flowers; standing clean rose flowers in stainless steel stirring equipment, adding five thousandths of biological enzyme A and biological enzyme B respectively, and stirring for 5min to be uniform; standing the uniformly stirred flowers in stainless steel coarse crushing equipment, and coarsely crushing the flowers into flower fragments less than or equal to 5 mm;

s2, placing the crushed rose into an extraction tray according to the height of 2cm, transferring into a quick-freezing warehouse, controlling the temperature of the quick-freezing warehouse at-50 ℃, and quickly freezing for 2 h. Heating a material partition plate in the low-temperature vacuum extraction bin to 41 ℃ while quickly freezing, and placing the quickly-frozen rose flowers on the material partition plate;

s3, controlling the pressure in the low-temperature vacuum extraction bin between-0.09 MPa and-0.095 MPa, controlling the temperature of the condensation distributor at-50 ℃, and keeping the condition for 12h, in the low-temperature vacuum condensation bin, continuously gasifying the cell sap in the rose flowers on the material partition plate, volatilizing the aromatic rose molecules into air, condensing the aromatic rose molecules into ice crystals when the aromatic rose molecules are attached to the condensation distributor, almost completely gasifying and solidifying the cell sap in the rose flowers on the condensation distributor after 12h of extraction, and drying the rose flowers. Heating the condensation distributor to 55 ℃ after extraction, circulating for 2h until the aromatic molecule ice crystals in the bin are completely melted, and collecting the rose cell stock solution;

s4 placing the rose cell stock solution in a freezer at-18 deg.C, standing, quickly freezing for 48h, thawing at room temperature, mixing with 10 ton stainless steel storage tank,

s5 and filtering by using a 0.22um microporous filter membrane;

s6, placing the filtered rose cell stock solution in a refrigerator at 7 ℃ and standing at a low temperature for 60 days for alcoholization, and filtering with 800-mesh filter cloth after alcoholization to obtain the finished product of the Damascus rose cell solution.

Comparative example 1:

the difference from example 1 is that in this comparative example, the second step is to distill the enzyme-treated rose directly to extract rose liquid, and the first step is the same as example 1.

Comparative example 2:

the difference from example 1 is that in this comparative example, the second step was to directly subject the enzyme-treated rose flowers to vacuum extraction of rose liquid, and the first step was performed in the same manner as in example 1.

Table 1 shows data on the extraction rate of rose cellular fluid in examples 1 to 6 and comparative examples 1 to 2. It can be seen from table 1 that in examples 1-6, the extraction rate of the rose cellular fluid is above 96%, the extracted rose is purple red, the rose flower is not lost, no waste is generated in the whole extraction process, i.e., the rose cellular fluid is extracted, and the complete rose flower can be obtained, so that the utilization rate of the rose flower is greatly improved, and the production cost of enterprises is reduced. In addition, the content of rose essential oil in the extracts of examples 1 to 6 is 0.01% to 0.02%, which is higher than that extracted by the conventional extraction method.

TABLE 1 data relating to extracts of examples 1-6 and comparative examples 1-2

Table 2 shows the composition data of the rose sap in examples 1 to 6 and comparative examples 1 to 2. As can be seen from Table 2, the cell sap extracted in examples 1-6 has less contents of ethanol and alpha-terpineol, but more contents of citronellol, nerol and geraniol than those in comparative examples 1-2, because the heating temperature for extracting the rose cell sap is low, the loss of alcohol aromatic components is less, the vacuum degree is high, and the volatile aromatic components in the rose are completely extracted in examples 1-6; the fresh flower is treated by biological enzyme catalysis and pulverization, so that the aromatic components in the fresh flower are well released, and the alcohol aromatic components are promoted to increase under the combined action of low temperature, high vacuum degree and enzyme treatment.

TABLE 2 extraction Components of examples 1-6 and comparative examples 1-2

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.