A kind of white orchid flower cell extract and supercritical extraction method

Abstract

The invention relates to the technical field of extraction, and in particular to a white orchid flower cell extract and a supercritical extraction method, comprising the following steps: (1) selecting white orchid flowers for standby use; (2) obtaining crushed materials; mixing the crushed materials with modified nanomaterials, and performing mixed grinding treatment; (3) drying the extractant carbon dioxide gas; (4) liquefying the carbon dioxide, and pressurizing the liquid carbon dioxide to a supercritical state; (5) obtaining a supercritical carbon dioxide fluid containing white orchid flower cell fluid; and (6) introducing the supercritical carbon dioxide fluid containing the white orchid flower cell fluid into a separation kettle, and completing extraction by decompression separation. The white orchid flower cell extract prepared by the invention is a natural product extracted from white orchid flowers and having multiple functions, and contains multiple chemical components, mainly including: linalool, 2-methylbutyric acid methyl ester, 2-methylbutyric acid, eugenol methyl ether, ethylene oxide methanol and other active ingredients.

Description

Technical Field

[0001] The invention relates to the technical field of extraction, in particular to a white orchid flower cell extract and a supercritical extraction method. Background Art

[0002] The liquid in the vacuole of plant cells is called cell sap. Cell sap is hypertonic, so plant cells can always be in a state of fullness. Anthocyanins in cell sap are related to the color of plants. The purple and deep red colors of flowers, fruits and leaves are determined by anthocyanins. Plant cell sap is also the living water that breeds plant life. It contains essential nutrients for maintaining plant life, such as inorganic salts, sugars, polyphenols, anthocyanins, vitamins, minerals and other active ingredients, as well as plant essential oils.

[0003] The cell sap is a complex aqueous solution consisting of endosomal fluid: all the fluid inside the cell, and exosomal fluid: all the fluid outside the cell; it has natural antimicrobial properties that plants use to protect themselves from pathogens.

[0004] Highly concentrated cell fluid nutrients and aromatherapy ingredients can fully exert stress relief, nourishing, beauty and anti-aging effects, improve negative emotions, skin sagging, dullness, wrinkles, spots, etc.

[0005] Steam distillation is the main method for obtaining most cell extracts on the market. However, steam distillation releases plant active ingredients into water, which will lose some aroma and even reduce the quality of the cell extract.

[0006] Based on this, the present invention provides a white orchid flower cell extract and a supercritical extraction method to obtain a cell extract with better performance. Summary of the invention

[0007] In view of the problems existing in the prior art, the present invention provides a white orchid flower cell extract and a supercritical extraction method.

[0008] To achieve the above object, the present invention provides the following technical solutions:

[0009] A supercritical extraction method for fresh flower cells of white orchid comprises the following steps:

[0010] (1) Select fresh, pest-free, fragrant white orchid flowers for later use;

[0011] (2) pre-crushing the fresh white orchid flowers obtained above to obtain crushed material;

[0012] The crushed material is mixed with the modified nanomaterial, and the mixed grinding process is performed for 2-3 hours;

[0013] Among them, the mixing mass ratio of crushed material and modified nanomaterial is 10:1-1.5;

[0014] (3) drying the extractant carbon dioxide gas;

[0015] (4) adding the crushed white jasmine flower material into the extraction kettle, turning on the refrigeration system to liquefy the carbon dioxide, and then pressurizing the liquid carbon dioxide to a supercritical state through a high-pressure pump;

[0016] (5) introducing the supercritical carbon dioxide into an extraction kettle and performing a step-by-step extraction process to obtain a supercritical carbon dioxide fluid containing the cell fluid of the fresh flower of the white orchid;

[0017] (6) The supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers is introduced into a separation kettle, and the extraction is completed by decompression separation.

[0018] As a further technical solution, the modified nanomaterial preparation method comprises:

[0019] First, nano-diatomite was added into deionized water, and then ultrasonically dispersed for 10 min to obtain nano-diatomite dispersion.

[0020] Maleic anhydride was added to the nano-diatomite dispersion, and the temperature was adjusted to be stable at 45°C, and the dispersion was stirred in a water bath for 30 minutes. Then the temperature was adjusted to 60°C and kept warm for 10 minutes. Sodium dodecyl sulfate and aspartic acid were added, and stirring was continued for 4 hours. Then, high-speed centrifugation was performed, suction filtration was performed, and low-temperature drying was performed to obtain modified nanomaterials.

[0021] As a further technical solution, the mixing ratio of the nano-diatomaceous earth and deionized water is 20-25 g: 200 mL;

[0022] The mixing ratio of maleic anhydride and nano-diatomite dispersion is 6-8g:200mL;

[0023] The mixing ratio of sodium dodecylbenzoate sulfonate, aspartic acid and nano-diatomaceous earth dispersion is 2-3g: 1-1.5g: 200mL.

[0024] As a further technical solution, the high-speed centrifugal treatment speed is 6000r / min;

[0025] The high-speed centrifugation treatment time was 15 min;

[0026] The low-temperature drying temperature is 55°C and the time is 20 hours.

[0027] As a further technical solution, the mixing and grinding speed is 800r / min;

[0028] The mixing and grinding time was carried out at room temperature and under an inert atmosphere;

[0029] The inert atmosphere is a nitrogen atmosphere.

[0030] As a further technical solution, the extraction agent carbon dioxide gas is dried as follows:

[0031] Preheat the extractant carbon dioxide to 80°C, keep it warm, and then continue to pass it into a drying tube filled with activated carbon for drying;

[0032] Among them, the drying time is 40 minutes.

[0033] As a further technical solution, the stepwise extraction process is:

[0034] The parameters of the supercritical carbon dioxide are adjusted to an upward gradient, specifically including 4 levels of gradient: a first-level gradient of carbon dioxide in a supercritical state, a second-level gradient of carbon dioxide in a supercritical state, a third-level gradient of carbon dioxide in a supercritical state, and a fourth-level gradient of carbon dioxide in a supercritical state;

[0035] Among them, the first-level gradient supercritical state of carbon dioxide is: temperature 40°C, pressure 30MPa, flow rate 400mL / min;

[0036] The secondary gradient supercritical carbon dioxide is: temperature 40°C, pressure 40MPa, flow rate 400mL / min;

[0037] The three-stage gradient supercritical carbon dioxide is: temperature 40°C, pressure 50MPa, flow rate 200mL / min;

[0038] The four-level gradient supercritical carbon dioxide is as follows: temperature 40°C, pressure 60MPa, and flow rate 200mL / min.

[0039] As a further technical solution, the extraction time of the primary gradient supercritical carbon dioxide is 1 hour;

[0040] The extraction time of the secondary gradient supercritical carbon dioxide is 1 hour;

[0041] The extraction time of three-stage gradient supercritical carbon dioxide is 2 hours;

[0042] The extraction time of the four-stage gradient supercritical carbon dioxide is 2 hours;

[0043] Finally, the supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers obtained by the four extractions is combined.

[0044] As a further technical solution, the decompression separation is:

[0045] Reduce pressure to normal pressure.

[0046] A supercritical extraction method for fresh flower cells of P. glabra is disclosed to obtain a fresh flower cell extract.

[0047] The white orchid flower cell extract prepared by the present invention should be stored in a cool and dry place, avoiding direct sunlight and high temperature environment.

[0048] Compared with the prior art, the present invention has the following beneficial effects:

[0049] The white jasmine flower cell extract prepared by the invention is a natural product extracted from the white jasmine flower and has multiple functions. The extract contains multiple chemical components, mainly including: linalool, methyl 2-methylbutyrate, 2-methylbutyric acid, eugenol methyl ether, ethylene oxide methanol and other active ingredients.

[0050] The white orchid flower cell extract prepared by the present invention has multiple functions. The active ingredients contained in the white orchid flower cell extract can activate the cell regeneration function and promote the blood circulation of the skin. It also has strong effects on cell regeneration and rebalancing oil secretion of dry and aging skin, thereby restoring the skin to its rosy and shiny state. It also helps to replenish water, moisturize, remove yellowness and brighten the skin, can greatly improve the skin, is beneficial to the health management of the skin, and has a more obvious skin care effect.

[0051] The white orchid flower cell extract prepared by the present invention also has a strong emotion regulation function, mainly has an obvious regulating effect on human nerves, mainly can relieve tense emotions, can reduce pressure and anxiety, calm the mind, has a more obvious effect in relaxing anxious and tense nerves, and can reduce adverse symptoms such as insomnia, forgetfulness, anxiety, dreaminess, depression and insomnia.

[0052] The present invention can promote the breakage of white orchid flower cells and the outflow of cell fluid by mixing and grinding white orchid flower crushed material with modified nanomaterials, modifying the nanomaterials and then mixing and grinding with the white orchid flower crushed material, thereby laying an important foundation for subsequent supercritical extraction and improving subsequent extraction efficiency.

[0053] By adopting a step-by-step extraction process, the extraction efficiency can be greatly improved, and the types of chemically active ingredients in the obtained white orchid flower extract are greatly improved, enriching the efficacy of the white orchid flower extract. In addition, it has a longer lasting fragrance performance, delays the release of fragrance, can continue to act on the skin for a longer time, and maintain the fragrance for a long time.

[0054] The white orchid flower cell extract prepared by the present invention can be applied to skin care products and aromatherapy products. The skin care products include essences, creams, lotions, etc., which are mainly used to improve skin conditions; and the aromatherapy products include aromatherapy essential oils, aromatherapy candles, etc., which mainly relieve stress and improve mood through the aroma emitted. BRIEF DESCRIPTION OF THE DRAWINGS

[0055] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings required for describing the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other accompanying drawings can be obtained based on these accompanying drawings without paying creative work.

[0056] Figure 1 It is a curve chart of time and storage fragrance retention rate. DETAILED DESCRIPTION

[0057] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0058] The following are specific embodiments:

[0059] Example 1

[0060] A supercritical extraction method for fresh flower cells of white orchid comprises the following steps:

[0061] (1) Select fresh, pest-free, fragrant white orchid flowers for later use;

[0062] (2) pre-crushing the fresh white orchid flowers obtained above to obtain crushed material;

[0063] The crushed material and the modified nanomaterial are mixed and ground for 2 hours;

[0064] Among them, the mixing mass ratio of crushed material and modified nanomaterial is 10:1;

[0065] The modified nanomaterial preparation method comprises:

[0066] First, nano-diatomite was added into deionized water, and then ultrasonically dispersed for 10 min to obtain nano-diatomite dispersion.

[0067] Maleic anhydride is added to the nano-diatomite dispersion, and the temperature is adjusted to be stable at 45°C, and the dispersion is stirred in a water bath for 30 minutes. Then the temperature is adjusted to 60°C and kept warm for 10 minutes. Then sodium dodecyl sulfate and aspartic acid are added, and stirring is continued for 4 hours. Then, high-speed centrifugation is performed, suction filtration is performed, and low-temperature drying is performed to obtain modified nanomaterials. The high-speed centrifugation speed is 6000r / min; and the high-speed centrifugation time is 15 minutes.

[0068] The mixing ratio of nano-diatomaceous earth and deionized water is 20g:200mL;

[0069] The mixing ratio of maleic anhydride and nano-diatomite dispersion is 6g:200mL;

[0070] The mixing ratio of sodium dodecylbenzoate sulfonate, aspartic acid and nano-diatomaceous earth dispersion is 2g:1g:200mL.

[0071] The low-temperature drying temperature is 55°C and the time is 20 hours.

[0072] The mixing and grinding speed is 800r / min;

[0073] The mixing and grinding time was carried out at room temperature and under an inert atmosphere;

[0074] The inert atmosphere is a nitrogen atmosphere.

[0075] (3) drying the extractant carbon dioxide gas; drying the extractant carbon dioxide gas is as follows:

[0076] Preheat the extractant carbon dioxide to 80°C, keep it warm, and then continue to pass it into a drying tube filled with activated carbon for drying;

[0077] Among them, the drying time is 40 minutes.

[0078] (4) adding the crushed white jasmine flower material into the extraction kettle, turning on the refrigeration system to liquefy the carbon dioxide, and then pressurizing the liquid carbon dioxide to a supercritical state through a high-pressure pump;

[0079] (5) introducing the supercritical carbon dioxide into an extraction kettle and performing a step-by-step extraction process to obtain a supercritical carbon dioxide fluid containing the cell fluid of the fresh flower of the white orchid;

[0080] The stepwise extraction process is:

[0081] The parameters of the supercritical carbon dioxide are adjusted to an upward gradient, specifically including 4 levels of gradient: a first-level gradient of carbon dioxide in a supercritical state, a second-level gradient of carbon dioxide in a supercritical state, a third-level gradient of carbon dioxide in a supercritical state, and a fourth-level gradient of carbon dioxide in a supercritical state;

[0082] Among them, the first-level gradient supercritical state of carbon dioxide is: temperature 40°C, pressure 30MPa, flow rate 400mL / min;

[0083] The secondary gradient supercritical carbon dioxide is: temperature 40°C, pressure 40MPa, flow rate 400mL / min;

[0084] The three-stage gradient supercritical carbon dioxide is: temperature 40°C, pressure 50MPa, flow rate 200mL / min;

[0085] The four-level gradient supercritical carbon dioxide is as follows: temperature 40°C, pressure 60MPa, and flow rate 200mL / min.

[0086] The extraction time of the first-stage gradient supercritical carbon dioxide is 1 hour;

[0087] The extraction time of the secondary gradient supercritical carbon dioxide is 1 hour;

[0088] The extraction time of three-stage gradient supercritical carbon dioxide is 2 hours;

[0089] The extraction time of the four-stage gradient supercritical carbon dioxide is 2 hours;

[0090] Finally, the supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers obtained by the four extractions is combined.

[0091] (6) The supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers is introduced into a separation kettle, and the extraction is completed by reducing the pressure to normal pressure.

[0092] Using HA220-40-11 supercritical CO2 extraction device, Beijing Jinyang Wanda Technology Co., Ltd.; Example 2

[0093] A supercritical extraction method for fresh flower cells of white orchid comprises the following steps:

[0094] (1) Select fresh, pest-free, fragrant white orchid flowers for later use;

[0095] (2) pre-crushing the fresh white orchid flowers obtained above to obtain crushed material;

[0096] The crushed material and the modified nanomaterial are mixed and ground for 2.5 hours;

[0097] Among them, the mixing mass ratio of crushed material and modified nanomaterial is 10:1.2;

[0098] The modified nanomaterial preparation method comprises:

[0099] First, nano-diatomite was added into deionized water, and then ultrasonically dispersed for 10 min to obtain nano-diatomite dispersion.

[0100] Maleic anhydride is added to the nano-diatomite dispersion, and the temperature is adjusted to be stable at 45°C, and the dispersion is stirred in a water bath for 30 minutes. Then the temperature is adjusted to 60°C and kept warm for 10 minutes. Then sodium dodecyl sulfate and aspartic acid are added, and stirring is continued for 4 hours. Then, high-speed centrifugation is performed, suction filtration is performed, and low-temperature drying is performed to obtain modified nanomaterials. The high-speed centrifugation speed is 6000r / min; and the high-speed centrifugation time is 15 minutes.

[0101] The mixing ratio of nano-diatomaceous earth and deionized water is 22g:200mL;

[0102] The mixing ratio of maleic anhydride and nano-diatomite dispersion is 6.5 g: 200 mL;

[0103] The mixing ratio of sodium dodecylbenzoate sulfonate, aspartic acid, and nano-diatomaceous earth dispersion is 2.8 g:1.2 g:200 mL.

[0104] The low-temperature drying temperature is 55°C and the time is 20 hours.

[0105] The mixing and grinding speed is 800r / min;

[0106] The mixing and grinding time was carried out at room temperature and under an inert atmosphere;

[0107] The inert atmosphere is a nitrogen atmosphere.

[0108] (3) drying the extractant carbon dioxide gas; drying the extractant carbon dioxide gas is as follows:

[0109] Preheat the extractant carbon dioxide to 80°C, keep it warm, and then continue to pass it into a drying tube filled with activated carbon for drying;

[0110] Among them, the drying time is 40 minutes.

[0111] (4) adding the crushed white jasmine flower material into the extraction kettle, turning on the refrigeration system to liquefy the carbon dioxide, and then pressurizing the liquid carbon dioxide to a supercritical state through a high-pressure pump;

[0112] (5) introducing the supercritical carbon dioxide into an extraction kettle and performing a step-by-step extraction process to obtain a supercritical carbon dioxide fluid containing the cell fluid of the fresh flower of the white orchid;

[0113] The stepwise extraction process is:

[0114] The parameters of the supercritical carbon dioxide are adjusted to an upward gradient, specifically including 4 levels of gradient: a first-level gradient of carbon dioxide in a supercritical state, a second-level gradient of carbon dioxide in a supercritical state, a third-level gradient of carbon dioxide in a supercritical state, and a fourth-level gradient of carbon dioxide in a supercritical state;

[0115] Among them, the first-level gradient supercritical state of carbon dioxide is: temperature 40°C, pressure 30MPa, flow rate 400mL / min;

[0116] The secondary gradient supercritical carbon dioxide is: temperature 40°C, pressure 40MPa, flow rate 400mL / min;

[0117] The three-stage gradient supercritical carbon dioxide is: temperature 40°C, pressure 50MPa, flow rate 200mL / min;

[0118] The four-level gradient supercritical carbon dioxide is as follows: temperature 40°C, pressure 60MPa, and flow rate 200mL / min.

[0119] The extraction time of the first-stage gradient supercritical carbon dioxide is 1 hour;

[0120] The extraction time of the secondary gradient supercritical carbon dioxide is 1 hour;

[0121] The extraction time of three-stage gradient supercritical carbon dioxide is 2 hours;

[0122] The extraction time of the four-stage gradient supercritical carbon dioxide is 2 hours;

[0123] Finally, the supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers obtained by the four extractions is combined.

[0124] (6) The supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers is introduced into a separation kettle, and the extraction is completed by reducing the pressure to normal pressure.

[0125] Example 3

[0126] A supercritical extraction method for fresh flower cells of white orchid comprises the following steps:

[0127] (1) Select fresh, pest-free, fragrant white orchid flowers for later use;

[0128] (2) pre-crushing the fresh white orchid flowers obtained above to obtain crushed material;

[0129] The crushed material and the modified nanomaterial are mixed and ground for 3 hours;

[0130] Among them, the mixing mass ratio of crushed material and modified nanomaterial is 10:1;

[0131] The modified nanomaterial preparation method comprises:

[0132] First, nano-diatomite was added into deionized water, and then ultrasonically dispersed for 10 min to obtain nano-diatomite dispersion.

[0133] Maleic anhydride is added to the nano-diatomite dispersion, and the temperature is adjusted to be stable at 45°C, and the dispersion is stirred in a water bath for 30 minutes. Then the temperature is adjusted to 60°C and kept warm for 10 minutes. Then sodium dodecyl sulfate and aspartic acid are added, and stirring is continued for 4 hours. Then, high-speed centrifugation is performed, suction filtration is performed, and low-temperature drying is performed to obtain modified nanomaterials. The high-speed centrifugation speed is 6000r / min; and the high-speed centrifugation time is 15 minutes.

[0134] The mixing ratio of nano-diatomaceous earth and deionized water is 23g:200mL;

[0135] The mixing ratio of maleic anhydride and nano-diatomite dispersion is 7.5 g: 200 mL;

[0136] The mixing ratio of sodium dodecylbenzoate sulfonate, aspartic acid, and nano-diatomaceous earth dispersion is 2.8 g:1.2 g:200 mL.

[0137] The low-temperature drying temperature is 55°C and the time is 20 hours.

[0138] The mixing and grinding speed is 800r / min;

[0139] The mixing and grinding time was carried out at room temperature and under an inert atmosphere;

[0140] The inert atmosphere is a nitrogen atmosphere.

[0141] (3) drying the extractant carbon dioxide gas; drying the extractant carbon dioxide gas is as follows:

[0142] Preheat the extractant carbon dioxide to 80°C, keep it warm, and then continue to pass it into a drying tube filled with activated carbon for drying;

[0143] Among them, the drying time is 40 minutes.

[0144] (4) adding the crushed white jasmine flower material into the extraction kettle, turning on the refrigeration system to liquefy the carbon dioxide, and then pressurizing the liquid carbon dioxide to a supercritical state through a high-pressure pump;

[0145] (5) introducing the supercritical carbon dioxide into an extraction kettle and performing a step-by-step extraction process to obtain a supercritical carbon dioxide fluid containing the cell fluid of the fresh flower of the white orchid;

[0146] The stepwise extraction process is:

[0147] The parameters of the supercritical carbon dioxide are adjusted to an upward gradient, specifically including 4 levels of gradient: a first-level gradient of carbon dioxide in a supercritical state, a second-level gradient of carbon dioxide in a supercritical state, a third-level gradient of carbon dioxide in a supercritical state, and a fourth-level gradient of carbon dioxide in a supercritical state;

[0148] Among them, the first-level gradient supercritical state of carbon dioxide is: temperature 40°C, pressure 30MPa, flow rate 400mL / min;

[0149] The secondary gradient supercritical carbon dioxide is: temperature 40°C, pressure 40MPa, flow rate 400mL / min;

[0150] The three-stage gradient supercritical carbon dioxide is: temperature 40°C, pressure 50MPa, flow rate 200mL / min;

[0151] The four-level gradient supercritical carbon dioxide is as follows: temperature 40°C, pressure 60MPa, and flow rate 200mL / min.

[0152] The extraction time of the first-stage gradient supercritical carbon dioxide is 1 hour;

[0153] The extraction time of the secondary gradient supercritical carbon dioxide is 1 hour;

[0154] The extraction time of three-stage gradient supercritical carbon dioxide is 2 hours;

[0155] The extraction time of the four-stage gradient supercritical carbon dioxide is 2 hours;

[0156] Finally, the supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers obtained by the four extractions is combined.

[0157] (6) The supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers is introduced into a separation kettle, and the extraction is completed by reducing the pressure to normal pressure.

[0158] Example 4

[0159] A supercritical extraction method for fresh flower cells of white orchid comprises the following steps:

[0160] (1) Select fresh, pest-free, fragrant white orchid flowers for later use;

[0161] (2) pre-crushing the fresh white orchid flowers obtained above to obtain crushed material;

[0162] The crushed material and the modified nanomaterial are mixed and ground for 3 hours;

[0163] Among them, the mixing mass ratio of crushed material and modified nanomaterial is 10:1.5;

[0164] The modified nanomaterial preparation method comprises:

[0165] First, nano-diatomite was added into deionized water, and then ultrasonically dispersed for 10 min to obtain nano-diatomite dispersion.

[0166] Maleic anhydride is added to the nano-diatomite dispersion, and the temperature is adjusted to be stable at 45°C, and the dispersion is stirred in a water bath for 30 minutes. Then the temperature is adjusted to 60°C and kept warm for 10 minutes. Then sodium dodecyl sulfate and aspartic acid are added, and stirring is continued for 4 hours. Then, high-speed centrifugation is performed, suction filtration is performed, and low-temperature drying is performed to obtain modified nanomaterials. The high-speed centrifugation speed is 6000r / min; and the high-speed centrifugation time is 15 minutes.

[0167] The mixing ratio of nano diatomaceous earth and deionized water is 25g:200mL;

[0168] The mixing ratio of maleic anhydride and nano-diatomite dispersion is 8g:200mL;

[0169] The mixing ratio of sodium dodecylbenzoate sulfonate, aspartic acid and nano-diatomaceous earth dispersion is 3g:1.5g:200mL.

[0170] The low-temperature drying temperature is 55°C and the time is 20 hours.

[0171] The mixing and grinding speed is 800r / min;

[0172] The mixing and grinding time was carried out at room temperature and under an inert atmosphere;

[0173] The inert atmosphere is a nitrogen atmosphere.

[0174] (3) drying the extractant carbon dioxide gas; drying the extractant carbon dioxide gas is as follows:

[0175] Preheat the extractant carbon dioxide to 80°C, keep it warm, and then continue to pass it into a drying tube filled with activated carbon for drying;

[0176] Among them, the drying time is 40 minutes.

[0177] (4) adding the crushed white jasmine flower material into the extraction kettle, turning on the refrigeration system to liquefy the carbon dioxide, and then pressurizing the liquid carbon dioxide to a supercritical state through a high-pressure pump;

[0178] (5) introducing the supercritical carbon dioxide into an extraction kettle and performing a step-by-step extraction process to obtain a supercritical carbon dioxide fluid containing the cell fluid of the fresh flower of the white orchid;

[0179] The stepwise extraction process is:

[0180] The parameters of the supercritical carbon dioxide are adjusted to an upward gradient, specifically including 4 levels of gradient: a first-level gradient of carbon dioxide in a supercritical state, a second-level gradient of carbon dioxide in a supercritical state, a third-level gradient of carbon dioxide in a supercritical state, and a fourth-level gradient of carbon dioxide in a supercritical state;

[0181] Among them, the first-level gradient supercritical state of carbon dioxide is: temperature 40°C, pressure 30MPa, flow rate 400mL / min;

[0182] The secondary gradient supercritical carbon dioxide is: temperature 40°C, pressure 40MPa, flow rate 400mL / min;

[0183] The three-stage gradient supercritical carbon dioxide is: temperature 40°C, pressure 50MPa, flow rate 200mL / min;

[0184] The four-level gradient supercritical carbon dioxide is as follows: temperature 40°C, pressure 60MPa, and flow rate 200mL / min.

[0185] The extraction time of the first-stage gradient supercritical carbon dioxide is 1 hour;

[0186] The extraction time of the secondary gradient supercritical carbon dioxide is 1 hour;

[0187] The extraction time of three-stage gradient supercritical carbon dioxide is 2 hours;

[0188] The extraction time of the four-stage gradient supercritical carbon dioxide is 2 hours;

[0189] Finally, the supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers obtained by the four extractions is combined.

[0190] (6) The supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers is introduced into a separation kettle, and the extraction is completed by reducing the pressure to normal pressure.

[0191] Comparative Example 1: This comparative example is basically the same as Example 1, except that no mixing and grinding treatment is performed with the modified nanomaterial.

[0192] Comparative Example 2: This comparative example is basically the same as Example 1, except that the modified nanomaterial is replaced by unmodified nano diatomaceous earth.

[0193] Comparative Example 3: This comparative example is basically the same as Example 1, except that the gradient extraction process is replaced by a fixed extraction process:

[0194] Temperature 40°C, pressure 60MPa, flow rate 200mL / min.

[0195] test:

[0196] The chemical components in the samples of the embodiments and comparative examples were identified by gas chromatography-mass spectrometry (GC-MS):

[0197] Table 1

[0198] Chemical composition type Example 1 86 Example 2 86 Example 3 86 Example 4 86 Comparative Example 1 79 Comparative Example 2 83 Comparative Example 3 72

[0199] It can be seen from Table 1 that the white orchid flower cell extract obtained by the supercritical extraction method of the present invention has richer chemical components.

[0200] Taking Example 1 as a specific sample, further testing was performed on the contents of the five components with the highest contents:

[0201] Table 2

[0202] Chemical composition content% Linalool 66.03％ Methyl 2-methylbutyrate 6.71％ 2-Methylbutyric acid 3.09％ Eugenol methyl ether 2.52％ Ethylene oxide methanol 1.58％

[0203] It can be seen from Table 2 that the linalool content in the fresh flower cell extract obtained by the method of the present invention is the highest.

[0204] The XP-329IIIR portable odor sensor was used to measure the change in alcohol content in the samples of the embodiment and the comparative example as the inspection standard for the fragrance retention, and the initial alcohol content was used as the standard. Then, the change in alcohol content was detected after storage for 24 hours, and the fragrance retention rate was calculated.

[0205] Table 3

[0206] Fragrance retention rate% Example 1 90.3 Example 2 89.5 Example 3 89.2 Example 4 90.7 Comparative Example 1 85.5 Comparative Example 2 87.2 Comparative Example 3 80.6

[0207] It can be seen from Table 3 that the white orchid flower cell extract obtained by the method of the present invention has a higher fragrance retention performance.

[0208] Taking Example 1 as the basic sample, the changes in the fragrance retention rate of the white orchid flower cell extract at different times are compared, as shown in FIG. Figure 1 .

[0209] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A supercritical extraction method for fresh flower cells of white orchid, characterized in that: The following steps are involved: (1) Select fresh, pest-free, fragrant white orchid flowers for later use; (2) pre-crushing the fresh white orchid flowers obtained above to obtain crushed material; The crushed material is mixed with the modified nanomaterial, and the mixed grinding process is performed for 2-3 hours; Among them, the mixing mass ratio of crushed material and modified nanomaterial is 10:1-1.5; (3) drying the extractant carbon dioxide gas; (4) adding the crushed white jasmine flower material into the extraction kettle, turning on the refrigeration system to liquefy the carbon dioxide, and then pressurizing the liquid carbon dioxide to a supercritical state through a high-pressure pump; (5) introducing the supercritical carbon dioxide into an extraction kettle and performing a step-by-step extraction process to obtain a supercritical carbon dioxide fluid containing the cell fluid of the fresh flower of the white orchid; (6) The supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers is introduced into a separation kettle, and the extraction is completed by decompression separation.

2. The method for supercritical extraction of fresh flower cells of white orchid according to claim 1, characterized in that: The modified nanomaterial preparation method comprises: First, nano-diatomite was added into deionized water, and then ultrasonically dispersed for 10 min to obtain nano-diatomite dispersion. Maleic anhydride was added to the nano-diatomite dispersion, and the temperature was adjusted to be stable at 45°C, and the dispersion was stirred in a water bath for 30 minutes. Then the temperature was adjusted to 60°C and kept warm for 10 minutes. Sodium dodecyl sulfate and aspartic acid were added, and stirring was continued for 4 hours. Then, high-speed centrifugation was performed, suction filtration was performed, and low-temperature drying was performed to obtain modified nanomaterials.

3. The method for supercritical extraction of fresh flower cells of white orchid according to claim 2, characterized in that: The mixing ratio of the nano-diatomaceous earth and deionized water is 20-25 g: 200 mL; The mixing ratio of maleic anhydride and nano-diatomite dispersion is 6-8g:200mL; The mixing ratio of sodium dodecylbenzoate sulfonate, aspartic acid and nano-diatomaceous earth dispersion is 2-3g: 1-1.5g: 200mL.

4. The method for supercritical extraction of fresh flower cells of white orchid according to claim 3, characterized in that: The high-speed centrifugal treatment speed is 6000r / min; The high-speed centrifugation treatment time was 15 min; The low-temperature drying temperature is 55°C and the time is 20 hours.

5. The method for supercritical extraction of fresh flower cells of white jasmine according to claim 4, characterized in that: The mixing and grinding speed is 800r / min; The mixing and grinding time was carried out at room temperature and under an inert atmosphere; The inert atmosphere is a nitrogen atmosphere.

6. The method for supercritical extraction of fresh flower cells of white orchid according to claim 1, characterized in that: The step of drying the extractant carbon dioxide gas is as follows: Preheat the extractant carbon dioxide to 80°C, keep it warm, and then continue to pass it into a drying tube filled with activated carbon for drying; Among them, the drying time is 40 minutes.

7. The method for supercritical extraction of fresh flower cells of white jasmine according to claim 1, characterized in that: The step-by-step extraction process is as follows: The parameters of the supercritical carbon dioxide are adjusted to an upward gradient, specifically including 4 levels of gradient: a first-level gradient of carbon dioxide in a supercritical state, a second-level gradient of carbon dioxide in a supercritical state, a third-level gradient of carbon dioxide in a supercritical state, and a fourth-level gradient of carbon dioxide in a supercritical state; Among them, the first-level gradient supercritical state of carbon dioxide is: temperature 40°C, pressure 30MPa, flow rate 400mL / min; The secondary gradient supercritical carbon dioxide is: temperature 40°C, pressure 40MPa, flow rate 400mL / min; The three-stage gradient supercritical carbon dioxide is: temperature 40°C, pressure 50MPa, flow rate 200mL / min; The four-level gradient supercritical carbon dioxide is as follows: temperature 40°C, pressure 60MPa, and flow rate 200mL / min.

8. The method for supercritical extraction of fresh flower cells of white jasmine according to claim 7, characterized in that: The extraction time of the first-level gradient supercritical carbon dioxide is 1 hour; The extraction time of the secondary gradient supercritical carbon dioxide is 1 hour; The extraction time of three-stage gradient supercritical carbon dioxide is 2 hours; The extraction time of the four-stage gradient supercritical carbon dioxide is 2 hours; Finally, the supercritical carbon dioxide fluid containing the cell fluid of the white orchid flowers obtained by the four extractions is combined.

9. The method for supercritical extraction of fresh flower cells of white orchid according to claim 1, characterized in that: The decompression separation is: Reduce pressure to normal pressure.

10. The method for supercritical extraction of fresh flower cells of B. glabra according to claim 1 obtains a B. glabra fresh flower cell extract.

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