CN112048384A - Preparation method of sea buckthorn fruit oil flavor and sodium carboxylate and fruit flavor type furan flavor - Google Patents
Preparation method of sea buckthorn fruit oil flavor and sodium carboxylate and fruit flavor type furan flavor Download PDFInfo
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Abstract
The invention relates to the field of spices, and discloses a method for preparing green strong fruity spice from pure natural edible sea-buckthorn fruit oil. The method comprises the steps of taking seabuckthorn fruit oil and alcohol as raw materials, adding pyrogallic acid as an antioxidant, adding water and taking a sodium hydroxide-alcohol solution as an alkali, and performing saponification reaction to obtain hydrolysis products of the seabuckthorn fruit oil, namely sodium aliphatic carboxylate and glycerol, wherein the saponification reaction is irreversible, and the theoretical conversion rate is close to 100%. Then under the catalysis of Lewis acid/protonic acid, the carboxylate which is a strong alkali and weak acid product of S1 has the balance of acid and acid radical ions, and the acid and ethanol/methanol are subjected to esterification reaction to generate an ethyl ester/methyl esterification product. So that the acid radical is continuously converted into acid which reacts with alcohol to generate an esterification product. The product has strong fruit fragrance, good fragrance durability and pure fragrance. Only one-pot method is needed for two-step reaction, the preparation steps of the sea buckthorn fruit oil flavor are simple, the yield is high, and the separation and purification are easy. The fragrance type is suitable for being used as a blending component for post blending in high-grade fresh and sweet fruity fragrance type perfume.
Description
Technical Field
The invention belongs to the technical field of spices, and particularly relates to a preparation method of a sea buckthorn fruit oil spice, a sodium carboxylate and a fruit-flavor furan spice.
Background
The perfume increasingly becomes an essential product for people to seek high-quality life, and is widely applied to various industries such as cosmetics, daily necessities and the like. The modern women pursued high-quality and elegant life is still lack of perfume cosmetics taking perfume as precursor. The daily necessities are added with the spice auxiliary agent, and the fashion of quality life is gradually formed. This makes the use of perfumes more widespread and in greater demand. The fruity sea-buckthorn fruit oil spice is derived from edible sea-buckthorn fruit oil beneficial to human bodies, and reagents involved in the preparation process are all green and non-toxic or substances which can be completely removed in the preparation process. The main components of the perfume are ester compounds. The fruity sea-buckthorn fruit oil spice has sweet, fruity and flowery flavor, is natural and fresh in fragrance, and is perfectly blended with elegant and mellow fragrance. The fragrance is lasting, pure, light and not light, elegant and not popular. Also has pure fragrance for refreshing. The sea-buckthorn is mostly born in arid desert, and the fruits are golden and juicy, so the spice is named as desert gold juice.
The seabuckthorn fruit oil is rich in more than 100 bioactive components, has high nutritional and health-care values, and also has the effects of reducing blood fat, resisting ulcer, improving immunity, beautifying and the like in the aspect of clinical medicine. Has been developed into various commodities such as high-grade edible oil, health care skin care products and the like. But the seabuckthorn fruit oil has the special aromatic smell, but does not have the seabuckthorn fruit oil flavor. The invention develops an esterification method which is green and nontoxic and keeps the original fragrance of the seabuckthorn fruit oil aiming at the special fragrance of the seabuckthorn fruit oil. Provides a new branch with high added value for the development of the downstream spice flavor industry of the seabuckthorn fruit oil.
Disclosure of Invention
The purpose of the invention is as follows: in order to provide a preparation method of sea buckthorn fruit oil flavor and carboxylic acid sodium salt and fruit flavor type furan flavor with better effect, the specific purpose is seen in a plurality of substantial technical effects of the specific implementation part.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for synthesizing a sea buckthorn fruit oil spice with fruit fragrance comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
Adding 1.0-1.2g of sea buckthorn fruit oil sample and 0.1-0.15g of pyrogallic acid antioxidant into a 100mL round bottom flask, adding magnetons, adding 2mL of ethanol with the mass fraction of 95% or methanol solution with the mass fraction of 99.5%, and 4mL of water, and uniformly stirring the magnetons. Then 8mL of ethanol or methanol solution of sodium hydroxide with the mass fraction of 2 percent is added, the spherical reflux condenser tube is connected, reflux is carried out on water bath at the temperature of 80 +/-1 ℃, and magnetic stirring is carried out at the rotating speed of 110 r/min. Until the oil drops disappear, the oil drops take 1 to 2 hours. The sea buckthorn fruit oil is saponified to produce intermediate sodium carboxylate as much as possible.
Second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in water bath at 80 +/-1 ℃, adding Lewis acid or protonic acid catalyst, 7mL of ethanol with the mass fraction of 95% or methanol with the mass fraction of 99.5% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water. The heating was stopped, the round bottom flask was removed from the water bath and the water bath was rapidly cooled to room temperature.
Extracting with 45mL petroleum ether or n-heptane for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times to remove inorganic substances and boron trifluoride etherate solution, washing with 30mL saturated salt water for 3 times, adding activated carbon with mass fraction of 16% and 200 meshes, stirring in 80 + -1 deg.C water bath for 30min to decolorize (noble and elegant light amber color), drying with anhydrous sodium sulfate, filtering, and concentrating to obtain fructus Hippophae oil essence containing ethyl myristate, ethyl palmitate, ethyl stearate, ethyl oleate, ethyl linoleate, and ethyl linolenate as main ingredients.
Further, in the first step, ethanol with a mass fraction of 95% or methanol with a mass fraction of 99.5% is selected for the ethyl esterification or methyl esterification.
Further, in the second step, a Lewis acid catalyst is selected from a boron trifluoride-methanol solution with a mass fraction of 14% or a boron trifluoride-diethyl ether solution with a mass fraction of 95%.
Further, in the second step, 1M hydrochloric acid solution is selected as the protonic acid catalyst.
Further, in the second step, petroleum ether or n-heptane is selected as the extractant.
Further, in the second step, activated carbon with the mass fraction of 16 percent and the particle size of 200 meshes is selected and added, and the mixture is stirred in a water bath at the temperature of 80 +/-1 ℃ for 30min to be decolorized.
Compared with the prior art, the invention adopting the technical scheme has the following beneficial effects: the invention provides a method for synthesizing a seabuckthorn fruit oil perfume with fruit fragrance, firstly, seabuckthorn fruit oil is subjected to saponification reaction in the presence of sodium hydroxide to obtain an intermediate seabuckthorn fruit oil carboxylic acid sodium salt, and then the carboxylic acid sodium salt is subjected to esterification reaction by using Lewis acid or protonic acid as a catalyst, so that the yield of the obtained esterified product is higher than 98%. Decoloring with 16% active carbon to change the perfume from dark red to amber yellow, with decoloring yield of 99.1%. Only one-pot method is needed for two-step reaction, the synthetic steps of the spice are simple, the separation and purification are easy, the solvent can be ethanol or n-heptane, and the spice keeps the special fruit aroma of the sea buckthorn and can be applied to spice, perfume or spice auxiliary agents.
Drawings
To further illustrate the present invention, further description is provided below with reference to the accompanying drawings:
FIG. 1 is a chemical diagram of the preparation of this patent;
FIG. 2 shows a spectrum analysis.
Detailed Description
The invention only needs a one-pot method for two-step reaction, the synthesis steps of the spice are simple, the separation and the purification are easy, and the prepared fruity type seabuckthorn fruit oil spice contains ester functional groups, so that the prepared fruity type seabuckthorn fruit oil spice has strong fruity flavor;
the technical solutions in the embodiments of the present invention will be clearly and completely described below, and the described embodiments are only a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
1.0141g of sea buckthorn fruit oil sample and 0.1056g of pyrogallic acid are added into a 100mL round-bottom flask, magnetons are added, 2mL of ethanol with the mass fraction of 95% and 4mL of water are added, and the magnetons are stirred uniformly. Then 8mL of ethanol solution with the mass fraction of 2 percent of sodium hydroxide is added, the mixture is connected with a spherical reflux condenser tube and refluxed in a water bath at the temperature of 80 ℃, and the magnetic stirring is carried out at the rotating speed of 110 r/min. Until the oil droplets disappeared, it took 1.5 hours. The sea buckthorn fruit oil is saponified to produce intermediate sodium carboxylate.
Second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in water bath at 80 ℃, adding 7.8mL of 1M hydrochloric acid solution and 7mL of ethanol with the mass fraction of 95% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water. The heating was stopped, the round bottom flask was removed from the water bath and the water bath was rapidly cooled to room temperature.
Extracting with 45mL petroleum ether for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 1.014g of the etherized fructus Hippophae oil essence with a yield of 99.36%. Adding 30% of active carbon with the mass fraction of 200 meshes, stirring in a water bath at 80 ℃ for 30min for decolorization, wherein the decolorization yield is 99.01%.
Example 2
A synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
1.0509g of sea buckthorn fruit oil sample and 0.1052g of pyrogallic acid are added into a 100mL round-bottom flask, magnetons are added, 2mL of 95% ethanol and 4mL of water are added, and the magnetons are stirred uniformly. Then 8mL of ethanol solution with the mass fraction of 2 percent of sodium hydroxide is added, the mixture is connected with a spherical reflux condenser tube and refluxed in a water bath at the temperature of 80 ℃, and the magnetic stirring is carried out at the rotating speed of 110 r/min. Until the oil droplets disappeared, it took 2 hours. The sea buckthorn fruit oil is saponified to produce intermediate sodium carboxylate.
Second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in water bath at 80 ℃, adding 7.8mL of 1M hydrochloric acid solution and 7mL of ethanol with the mass fraction of 95% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water. The heating was stopped, the round bottom flask was removed from the water bath and the water bath was rapidly cooled to room temperature.
Then extracting with 45mL of n-heptane for 3 times, combining organic phases, washing with 30mL of distilled water for 3 times, washing with 30mL of saturated salt solution for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 1.0161g of the etherized seabuckthorn fruit oil spice with the yield of 96.68%. Adding 30% of active carbon with the mass fraction of 200 meshes, stirring in a water bath at 80 ℃ for 30min, and decoloring, wherein the decoloring yield is 98.93%.
Example 3
A synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
1.0381g of sea buckthorn fruit oil sample and 0.1087g of pyrogallic acid are added into a 100mL round-bottom flask, magnetons are added, 2mL of methanol with the mass fraction of 95% and 4mL of water are added, and the magnetons are stirred uniformly. Then 8mL of methanol solution with 2 percent of sodium hydroxide by mass fraction is added, the mixture is connected with a spherical reflux condenser tube and refluxed on a water bath at the temperature of 80 ℃, and the magnetic stirring is carried out at the rotating speed of 110 r/min. Until the oil droplets disappeared, it took 1.5 hours. The sea buckthorn fruit oil is saponified to produce intermediate sodium carboxylate.
Second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in water bath at 80 ℃, adding 7mL of 14% boron trifluoride-methanol solution from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water. The heating was stopped, the round bottom flask was removed from the water bath and the water bath was rapidly cooled to room temperature.
Then extracting with 45mL n-heptane for 3 times, combining organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 0.9934g methyl esterified fructus Hippophae oil perfume with a yield of 95.69%. Adding 30% of active carbon with the mass fraction of 200 meshes, stirring in a water bath at 80 ℃ for 30min, and decoloring, wherein the decoloring yield is 99.20%.
Example 4
A synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
1.0302g of sea buckthorn fruit oil sample and 0.1029g of pyrogallic acid are added into a 100mL round-bottom flask, magnetons are added, 2mL of ethanol with the mass fraction of 95% and 4mL of water are added, and the magnetons are stirred uniformly. Then 8mL of ethanol solution with the mass fraction of 2 percent of sodium hydroxide is added, the mixture is connected with a spherical reflux condenser tube and refluxed in a water bath at the temperature of 80 ℃, and the magnetic stirring is carried out at the rotating speed of 110 r/min. Until the oil droplets disappeared, it took 1.5 hours. The sea buckthorn fruit oil is saponified to produce intermediate sodium carboxylate.
Second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in water bath at 80 ℃, adding 1.2mL of boron trifluoride-diethyl ether solution with the mass fraction of 95% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water. The heating was stopped, the round bottom flask was removed from the water bath and the water bath was rapidly cooled to room temperature.
Extracting with 45mL petroleum ether for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 1.0285g of the etherized fructus Hippophae oil perfume with a yield of 99.83%. Adding 30% of fructus Hippophae oil and active carbon with particle size of 200 meshes, stirring in 80 deg.C water bath for 30min for decolorizing with decolorizing yield of 99.07%.
Product fragrance test
Respectively using boron trifluoride methanol as acid methyl esterification product A, hydrochloric acid as acid ethyl esterification product B and boron trifluoride diethyl etherate as ethyl esterification product C, and respectively using ethanol and n-heptane as different solvents. Concentration of C when not diluted0When diluted 10 times, the concentration is C 120 times the concentration of C2At 40 times, the concentration is C380 times the concentration of C4The perfume samples with different concentrations are dipped in clean and tasteless perfume testing paper, and the perfume is tested in a laboratory with fresh air and no interference of other odors, and the grades are divided into a superior grade, a superior grade and a superior grade.
The flavors of the esterified seabuckthorn fruit oil spice and the ethylenated seabuckthorn fruit oil spice are not obviously different; ethanol and n-heptane are used as solvents, and the fragrance of the n-heptane is more suitable for the fragrance of the sea buckthorn fruit oil fragrance than the ethanol; the dilution concentration of the perfume is 10-20 times, the aroma is moderate, and the aroma is better in embodiment.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are intended to illustrate the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and the invention is to be limited to the embodiments described above.
Claims (9)
1. The sea buckthorn fruit oil flavor is characterized by comprising any one or more of the following three substances;
R1，R2，R3＝C17H35，C13H27，C15H29，C15H31，C17H33，C17H31，C17H29
R＝CH3，C2H5。
2. the intermediate sodium salt of seabuckthorn fruit oil carboxylic acid prepared from seabuckthorn fruit oil spice is characterized by comprising any one or more of the following three substances;
R1，R2，R3＝C17H35，C13H27，C15H29，C15H31，C17H33，C17H31，C17H29。
3. a method for preparing green strong fruity flavor spice from pure natural edible sea-buckthorn fruit oil is characterized by adopting a one-pot method and two-step reaction:
s1 saponification of sea buckthorn fruit oil: taking seabuckthorn fruit oil and alcohol as raw materials, adding pyrogallic acid as an antioxidant, adding water and taking a sodium hydroxide-alcohol solution as an alkali, and performing saponification reaction to obtain hydrolysis products of the seabuckthorn fruit oil, namely sodium aliphatic carboxylate and glycerol;
secondly, under the catalysis of Lewis acid/protonic acid, the carboxylate which is a strong-base weak-acid product of S1 has the balance of acid and acid radical ions, and the acid and ethanol/methanol generate esterification reaction to generate an ethyl ester/methyl esterification product, so that the acid radical is continuously converted into the acid to react with the alcohol to generate the esterification product; the product has strong fruit fragrance, good fragrance durability and pure fragrance.
4. The method for preparing green full-bodied fruity flavor from pure natural edible seabuckthorn fruit oil according to claim 3, wherein the method for synthesizing the seabuckthorn fruit oil flavor with fruity flavor comprises the following steps:
the preparation method of the sea buckthorn fruit oil flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
Adding 1.0-1.2g of sea buckthorn fruit oil sample and 0.1-0.15g of pyrogallic acid antioxidant into a 100mL round bottom flask, adding magnetons, adding 2mL of ethanol with the mass fraction of 95% or a methanol solution with the mass fraction of 99.5% and 4mL of water, and uniformly stirring the magnetons; then 8mL of ethanol or methanol solution of sodium hydroxide with the mass fraction of 2 percent is added, a spherical reflux condenser tube is connected, reflux is carried out on a water bath at the temperature of 80 +/-1 ℃, and magnetic stirring is carried out at the rotating speed of 110 r/min; until the oil drops disappear, the use time is 1 to 2 hours; the saponification reaction of the seabuckthorn fruit oil is as thorough as possible;
second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in water bath at 80 +/-1 ℃, adding Lewis acid or protonic acid catalyst and 7mL of ethanol with the mass fraction of 95% or methanol with the mass fraction of 99.5% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water; stopping heating, taking off the round-bottom flask from the water bath, and rapidly cooling to room temperature in the water bath; extracting with 45mL petroleum ether or n-heptane for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times to remove inorganic substances and Lewis acid solution, washing with 30mL saturated salt water for 3 times, adding activated carbon with mass fraction of 16% and 200 meshes, stirring in 80 + -1 deg.C water bath for 30min for decolorization, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain fructus Hippophae oil essence containing ethyl myristate, ethyl palmitate, ethyl stearate, ethyl oleate, ethyl linoleate, and ethyl linolenate as main ingredients.
5. The method of claim 4, wherein in the first step pyrogallic acid is added as an antioxidant; 2mL of ethanol with the mass fraction of 95% or methanol solution with the mass fraction of 99.5% is used as a phase transfer solvent.
6. The method of claim 4, wherein in the first step, 8mL of 2% sodium hydroxide ethanol or methanol is added as alkali; the reaction was heated in a water bath until the oil droplets disappeared.
7. The method of claim 4, wherein in the second step, adding Lewis acid means adding 1.2mL of 95% by weight boron trifluoride etherate; the addition of the protonic acid catalyst means that 7.8mL of 1M aqueous hydrochloric acid solution was added.
8. The method of claim 4, wherein in the second step, 7mL of 95% by weight ethanol or 99.5% by weight methanol solution is added; in the second step, refluxing was continued for 20 min.
9. A method for synthesizing furan perfume with fruity flavor is characterized by adopting any one of the following schemes:
firstly, the method comprises the following steps: a synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
Adding 1.0141g of sea buckthorn fruit oil sample and 0.1056g of pyrogallic acid into a 100mL round-bottom flask, adding magnetons, then adding 2mL of ethanol with the mass fraction of 95% and 4mL of water, and uniformly stirring the magnetons; then 8mL of ethanol solution with the mass fraction of 2% of sodium hydroxide is added, the mixture is connected with a spherical reflux condenser tube, reflux is carried out on a water bath at the temperature of 80 ℃, and magnetic stirring is carried out at the rotating speed of 110 r/min; until the oil drops disappear, the use time is 1.5 hours; performing saponification reaction on the seabuckthorn fruit oil to generate an intermediate sodium carboxylate;
second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in a water bath at 80 ℃, adding 7.8mL of 1M hydrochloric acid solution and 7mL of ethanol with the mass fraction of 95% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water; stopping heating, taking off the round-bottom flask from the water bath, and rapidly cooling to room temperature in the water bath;
extracting with 45mL petroleum ether for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 1.014g of ethyl ester-type fructus Hippophae oil essence with a yield of 99.36%; adding 30% of active carbon with the mass fraction of 200 meshes, stirring in a water bath at 80 ℃ for 30min for decolorization, wherein the decolorization yield is 99.01%;
II, secondly: a synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
Adding 1.0509g of sea buckthorn fruit oil sample and 0.1052g of pyrogallic acid into a 100mL round-bottom flask, adding magnetons, then adding 2mL of ethanol with the mass fraction of 95% and 4mL of water, and uniformly stirring the magnetons; then 8mL of ethanol solution with the mass fraction of 2% of sodium hydroxide is added, the mixture is connected with a spherical reflux condenser tube, reflux is carried out on a water bath at the temperature of 80 ℃, and magnetic stirring is carried out at the rotating speed of 110 r/min; until the oil drops disappear, the oil drops are used for 2 hours; performing saponification reaction on the seabuckthorn fruit oil to generate an intermediate sodium carboxylate;
second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in a water bath at 80 ℃, adding 7.8mL of 1M hydrochloric acid solution and 7mL of ethanol with the mass fraction of 95% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water; stopping heating, taking off the round-bottom flask from the water bath, and rapidly cooling to room temperature in the water bath;
extracting with 45mL n-heptane for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 1.0161g of the etherized fructus Hippophae oil perfume with a yield of 96.68%; adding 30% of active carbon with the mass fraction of 200 meshes, stirring in a water bath at 80 ℃ for 30min for decolorization, wherein the decolorization yield is 98.93%;
thirdly, the method comprises the following steps: a synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
Adding 1.0381g of sea buckthorn fruit oil sample and 0.1087g of pyrogallic acid into a 100mL round-bottom flask, adding magnetons, then adding 2mL of methanol with the mass fraction of 95% and 4mL of water, and uniformly stirring the magnetons; then adding 8mL of methanol solution of sodium hydroxide with the mass fraction of 2%, connecting a spherical reflux condenser tube, refluxing on a water bath at the temperature of 80 ℃, and magnetically stirring at the rotating speed of 110 r/min; until the oil drops disappear, the use time is 1.5 hours; performing saponification reaction on the seabuckthorn fruit oil to generate an intermediate sodium carboxylate;
second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in a water bath at 80 ℃, adding 7mL of boron trifluoride-methanol solution with the mass fraction of 14% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water; stopping heating, taking off the round-bottom flask from the water bath, and rapidly cooling to room temperature in the water bath;
extracting with 45mL n-heptane for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 0.9934g methyl esterified fructus Hippophae oil perfume with yield of 95.69%; adding 30% of active carbon with the mass fraction of 200 meshes, stirring in a water bath at 80 ℃ for 30min, and decoloring, wherein the decoloring yield is 99.20%;
fourthly, the method comprises the following steps: a synthetic method of furan flavor with fruity flavor comprises the following steps:
first step, preparation of intermediate sodium salt of seabuckthorn fruit oil carboxylic acid
Adding 1.0302g of sea buckthorn fruit oil sample and 0.1029g of pyrogallic acid into a 100mL round-bottom flask, adding magnetons, then adding 2mL of ethanol with the mass fraction of 95% and 4mL of water, and uniformly stirring the magnetons; then 8mL of ethanol solution with the mass fraction of 2% of sodium hydroxide is added, the mixture is connected with a spherical reflux condenser tube, reflux is carried out on a water bath at the temperature of 80 ℃, and magnetic stirring is carried out at the rotating speed of 110 r/min; until the oil drops disappear, the use time is 1.5 hours; performing saponification reaction on the seabuckthorn fruit oil to generate an intermediate sodium carboxylate;
second step, synthesis of sea buckthorn fruit oil flavor
Keeping the reflux pipe heated in a water bath at 80 ℃, adding 1.2mL of boron trifluoride-diethyl ether solution with the mass fraction of 95% from the upper end of the reflux condenser pipe, continuously refluxing for 20min, and washing the reflux condenser pipe with a small amount of water; stopping heating, taking off the round-bottom flask from the water bath, and rapidly cooling to room temperature in the water bath;
extracting with 45mL petroleum ether for 3 times, mixing organic phases, washing with 30mL distilled water for 3 times, washing with 30mL saturated salt water for 3 times, drying with anhydrous sodium sulfate, filtering, and concentrating to obtain 1.0285g of the etherized fructus Hippophae oil perfume with a yield of 99.83%; adding 30% of fructus Hippophae oil and active carbon with particle size of 200 meshes, stirring in 80 deg.C water bath for 30min for decolorizing with decolorizing yield of 99.07%.
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