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CN-121975581-A - Preparation method of peony lavender blend essential oil

CN121975581ACN 121975581 ACN121975581 ACN 121975581ACN-121975581-A

Abstract

The invention belongs to the technical field of extraction and blending of natural plant essential oil, and discloses a preparation method of peony lavender blend essential oil. The method is characterized by comprising the steps of mixing peony petals with lavender ears, pretreating by a complex enzyme system, sequentially carrying out gradient separation by a three-stage bionic membrane, and combining vacuum low-temperature distillation to realize efficient extraction and enrichment of volatile esters, aromatic alcohols and functional precursor substances at low temperature. According to the invention, by constructing a low-temperature extraction scheme of enzyme-membrane cooperation, not only is synchronous and efficient extraction of volatile, thermosensitive and functional multidimensional components in the peony and lavender composite essential oil realized, but also the molecular recognition capability of the bionic membrane is utilized to endow the product with higher component purity, fragrance fidelity and biological activity value, and a brand new scheme is provided for green and accurate manufacture of high-end natural composite essential oil.

Inventors

  • LUO DONGMING
  • Guo Houlang

Assignees

  • 江西海瑞天然植物有限公司

Dates

Publication Date
20260505
Application Date
20260319

Claims (10)

  1. 1. The preparation method of the peony lavender blend essential oil is characterized by comprising the following steps of: Mixing the peony petals dried until the water content is lower than 8% with the lavender flower ears according to the mass ratio of 1:1-3:1, and crushing to obtain mixed plant powder; Adding deionized water with the mass 3-5 times of that of the mixed plant powder, and regulating the pH value to 4.8-5.2 to form suspension; Sequentially adding cellulase, pectase and hemicellulase into the suspension, wherein the mass ratio of the cellulase to the pectase to the hemicellulase is 2:1:1, the total enzyme addition amount is 0.8% -1.2% of the mass of the mixed plant powder, and performing constant-temperature oscillation reaction at 35+/-2 ℃ to complete enzymolysis pretreatment to obtain enzymolysis liquid; performing primary solid-liquid separation on the enzymolysis liquid through a stainless steel filter screen with the aperture of 50 mu m to obtain clear filtrate; sequentially passing the clarified filtrate through three stages of bionic membrane separation units connected in series to obtain concentrated solution; and (3) carrying out vacuum low-temperature distillation on the concentrated solution at 35 ℃ under absolute pressure of less than or equal to 5kPa, and removing residual moisture to obtain the peony lavender blend essential oil.
  2. 2. The preparation method according to claim 1, wherein the clear filtrate sequentially passes through three stages of biomimetic membrane separation units connected in series specifically comprises: the first stage adopts a polyethersulfone-phospholipid bilayer composite ultrafiltration membrane with a molecular weight cutoff of 100kDa, and operates under the operating pressure of 0.15-0.20MPa to intercept macromolecular impurities and obtain a first stage permeate; The second stage adopts a polyvinylidene fluoride-cholesterol segmented copolymer nanofiltration membrane with a cut-off molecular weight of 10kDa, and operates under the operating pressure of 0.30-0.35MPa to cut-off flavonoid glycoside and phenolic acid precursor substances, so as to obtain a second-stage permeate; And thirdly, adopting a polyamide-phospholipid bionic reverse osmosis membrane with the molecular weight cutoff of 300Da, operating at the operating pressure of 0.8-1.0MPa, intercepting target aromatic components, and concentrating to obtain concentrated solution.
  3. 3. The preparation method according to claim 1, wherein the cellulase has an enzyme activity of more than 15000U/g, the pectase has an enzyme activity of more than 8000U/g, and the hemicellulase has an enzyme activity of more than 10000U/g.
  4. 4. A method according to claim 1 or 3, wherein the dissolved oxygen concentration is maintained at 2-4mg/L during the enzymatic hydrolysis reaction.
  5. 5. The preparation method of the polyether sulfone-phospholipid bilayer composite ultrafiltration membrane is characterized by comprising the steps of dissolving polyether sulfone in N-methylpyrrolidone to prepare a casting solution with the mass concentration of 18%, adding dipalmitoyl phosphatidylcholine accounting for 5% of the mass of the polyether sulfone, stirring uniformly, standing for deaeration, scraping a liquid film with the thickness of 120 mu m on a non-woven fabric supporting layer by using a scraper, immersing the liquid film in a deionized water coagulation bath for phase conversion to form a film, and then carrying out crosslinking treatment.
  6. 6. The preparation method of the polyvinylidene fluoride-cholesterol block copolymer nanofiltration membrane according to claim 2, wherein the polyvinylidene fluoride-cholesterol block copolymer nanofiltration membrane is prepared by in-situ polymerization, wherein polyvinylidene fluoride microspheres are dispersed in an ethanol-water mixed solvent, cholesterol glycidyl ether and hexamethylenediamine with a molar ratio of 1:1 are added for reaction, and cholesterol groups are covalently grafted on the surface of the membrane through amide bonds, so that a nanofiltration separation layer with lipid bilayer micro-regions is formed.
  7. 7. The preparation method of claim 6, wherein the retention rate of the polyvinylidene fluoride-cholesterol segmented copolymer nanofiltration membrane on flavonoid glycoside substances with the molecular weight of 1000-5000Da is more than or equal to 92%.
  8. 8. The preparation method of the bionic reverse osmosis membrane according to claim 2, wherein the bionic reverse osmosis membrane is prepared by interfacial polymerization, wherein m-phenylenediamine aqueous solution is used as an aqueous phase, trimesoyl chloride n-hexane solution is used as an oil phase, interfacial polymerization is carried out on a polysulfone ultrafiltration base membrane to form a polyamide separation layer, then the membrane is immersed in ethanol solution containing 1% lecithin, self-assembly is carried out for 1 hour at 30 ℃, and phospholipid molecules are aligned on the surface of the polyamide to form a bionic phospholipid monolayer with the thickness of about 5 nm.
  9. 9. The method according to claim 8, wherein the permeation flux of the polyamide-phospholipid biomimetic reverse osmosis membrane to water molecules is 25-30L/(m 2 .h.mpa), and the rejection rate to linalool is 98.5% or more.
  10. 10. The method according to claim 1, wherein the vacuum cryogenic distillation is performed by a wiped film molecular distillation apparatus having a rotor speed of 200 to 300rpm and a separation between the evaporation surface and the condensation surface of 30mm.

Description

Preparation method of peony lavender blend essential oil Technical Field The invention belongs to the technical field of extraction and blending of natural plant essential oil, and relates to a preparation method of peony lavender blend essential oil. Background The compound blend essential oil represented by the peony flowers and the lavender in the natural plant essential oil is increasingly favored by the high-end essence and spice market by virtue of the elegant and fragrant fragrance profile and the synergistic relaxing function. The steam distillation method is used as a classical means for extracting plant essential oil, volatile components are carried out by using steam, and oil-water separation is realized after condensation, so that target essential oil is obtained. The method has good applicability in treating high-temperature-resistant and high-volatility monoterpene compounds, and effectively solves the feasibility problem of large-scale extraction in the early stage of industrialization. The steam distillation process is usually carried out for tens of minutes to hours at the temperature of 95-100 ℃ or even higher, the high-temperature environment is extremely easy to cause the oxidation, isomerization or dehydration reaction of the heat-sensitive aromatic alcohols such as phenethyl alcohol, geraniol and the like which are rich in the peony, and meanwhile, the key linalool, linalyl acetate and other ester components in the lavender are easy to hydrolyze and inactivate, so that the obtained essential oil has distorted aroma, lost head fragrance and is more likely to lose part of pharmacological synergistic effect. Meanwhile, steam distillation depends on the volatility of components rather than the polarity or molecular size, a large amount of non-volatile but functionally valuable flavone and polyphenol precursor substances cannot be effectively extracted, so that the overall extraction rate is generally low, and is usually less than 30% of the total amount of soluble aromatic substances in raw materials, so that the valuable plant resources are wasted obviously. While attempts have been made to introduce alternatives such as supercritical CO 2 extraction, solvent leaching, etc., the former is expensive in equipment cost and has limited selectivity to polar components, while the latter suffers from solvent residue and subsequent purification problems, and it is difficult to achieve an ideal balance between cost, safety and component integrity. The cross fusion of enzyme engineering and bionic membrane separation technology provides a new idea for gently breaking plant cell wall barriers through a specific enzyme system, releasing intracellular aromatic precursors, and combining a separation medium simulating selective permeability of a biological membrane to realize accurate interception and concentration of target molecules under the condition of near normal temperature. Disclosure of Invention In order to achieve the aim of the invention, the invention provides a preparation method of peony lavender blend essential oil, which is characterized in that a low-temperature extraction system based on the synergistic effect of compound enzyme pretreatment and multi-stage bionic membrane gradient separation is constructed, and the high-efficiency, complete extraction and selective enrichment of thermosensitive aromatic alcohols, volatile esters and functional non-volatile precursor substances in peony and lavender raw materials are synchronously realized at the process temperature of lower than 40 ℃, so that the compound blend essential oil with high reduction of aroma profile, stable component structure, high bioactivity retention rate and remarkably improved yield is obtained. Firstly, mixing peony petals dried until the water content is lower than 8% with lavender ears according to the mass ratio of 1:1-3:1, and crushing the mixture to the particle size of 0.5-2.0mm to obtain mixed plant powder; adding deionized water with the mass of 3-5 times of that of the mixed plant powder to regulate the pH value to 4.8-5.2 to form suspension, sequentially adding cellulase, pectase and hemicellulase into the suspension, wherein the mass ratio of the cellulase to the pectase to the hemicellulase is 2:1:1, the total enzyme addition amount is 0.8-1.2% of that of the mixed plant powder, carrying out constant-temperature oscillation reaction for 90-120min at 35+/-2 ℃ to finish enzymolysis pretreatment, carrying out primary solid-liquid separation on the obtained enzymolysis liquid through a stainless steel filter screen with the aperture of 50 mu m after the enzymolysis is finished to obtain clear filtrate, sequentially passing through a three-stage serial bionic membrane separation unit, wherein the operation pressure, the interception molecular weight and the functional goal of each stage membrane unit are as follows, the first stage adopts a polyethersulfone-phospholipid double-molecular layer composite ultra