CN110079393B - Pearl blasting essential oil and preparation method and application thereof - Google Patents
Pearl blasting essential oil and preparation method and application thereof Download PDFInfo
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- CN110079393B CN110079393B CN201910354505.0A CN201910354505A CN110079393B CN 110079393 B CN110079393 B CN 110079393B CN 201910354505 A CN201910354505 A CN 201910354505A CN 110079393 B CN110079393 B CN 110079393B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/241—Extraction of specific substances
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0069—Heterocyclic compounds
- C11B9/0073—Heterocyclic compounds containing only O or S as heteroatoms
- C11B9/008—Heterocyclic compounds containing only O or S as heteroatoms the hetero rings containing six atoms
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses pearl blasting essential oil and a preparation method and application thereof. Taking the licorice extract to carry out esterification reaction; extracting the esterification product with ethyl acetate, mixing the upper layer extract with oil solvent such as caprylic capric acid glyceride and/or glyceryl monocaprylate, and removing solvent to obtain the exploder bead essential oil. The invention also discloses application of the bead blasting essential oil in preparing a bead blasting cigarette holder. The invention utilizes the liquorice extract to prepare the popping essential oil through esterification reaction products, has novel method and clear and definite main component types, and effectively relieves the discomfort of smoke to throat and lung.
Description
Technical Field
The invention belongs to the technical field of cigarette essence and spice addition, and particularly relates to bead blasting essential oil and a preparation method and application thereof.
Background
The puffing bead is a small capsule containing spice liquid embedded in a cigarette filter tip, also called as a fragrant pill, a brittle capsule and a bead, and according to the preference, a smoker puffs at any time in the smoking process, so that the cigarette has unique taste and comfortable experience due to different spice types.
Most of the pearl blasting essential oil in the market is prepared from various essential oils or extracted from various Chinese herbal medicines, and the pearl blasting essential oil has various raw materials and complex process.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems in the prior art, the invention provides popping pearl essential oil taking liquorice as a raw material and a preparation method thereof.
The technical scheme is as follows: a preparation method of bead blasting essential oil comprises the following steps: taking the licorice extract to carry out esterification reaction; extracting the esterification product with ethyl acetate, mixing the upper layer extract with a grease solvent, and removing the extraction solvent to obtain the exploded bead essential oil.
The Glycyrrhrizae radix extract is alcohol extract of Glycyrrhrizae radix.
The molecular weight of the main components in the liquorice is increased through esterification reaction, so that the liquorice is easy to extract and dissolve in grease, and the essential oil contains more effective components of the liquorice. The esterification method comprises the following steps: dissolving the licorice extract with alcohol, adding concentrated sulfuric acid, reacting for 2-5 h at 30-60 ℃, and removing supernatant to obtain an esterification product.
The esterification reaction solvent is absolute ethyl alcohol with the mass 2-5 times that of the licorice extract, the mass fraction of concentrated sulfuric acid is 5-20%, and the adding amount of the concentrated sulfuric acid is 1-2 times that of the licorice extract.
The esterification reaction conditions can be fast and fully completed.
During extraction, after the esterification product is dissolved by 6-10 times of mass of liquorice extract, ethyl acetate 4-10 times of mass of the liquorice extract is added for extraction, so that effective components are fully extracted.
The grease solvent is glyceryl monocaprylate or/and glyceryl caprylate/caprate, and the two kinds of grease have good dissolubility to the extract. Further, the grease solvent is a mixture of glyceryl monocaprylate and glyceryl caprylate-caprate in a ratio of 0-2: 1. The addition amount of the grease solvent is 6-8 times of the mass of the liquorice extract, the clarity is good, and the taste is proper.
The solvent can be removed by adding water, and bubbles are generated under heating and vacuum conditions by utilizing the property of oil-water incompatibility, so that the organic solvent can be removed better, the health of smokers is protected, and the production is more convenient.
The invention also provides the popping essential oil prepared by the preparation method.
The invention also provides application of the bead blasting essential oil in preparing a bead blasting cigarette holder.
The invention also provides a bead blasting cigarette holder which adopts the bead blasting essential oil.
Has the advantages that:
the liquorice is an important traditional Chinese medicine and is called by China and old people, and has the effects of eliminating phlegm and relieving cough. The invention utilizes the liquorice extract to prepare the popping essential oil through esterification reaction products, has novel method and clear and definite main component types, and effectively relieves the discomfort of smoke to throat and lung.
The liquorice contains a large amount of flavonoid compounds, most of which belong to chalcone and flavanone and contain 3 'and 4' hydroxyl, and phenolic hydroxyl compounds have an antioxidant function, and quench singlet oxygen atoms or eliminate free radicals to prevent peroxidation so that new hydrocarbon free radicals are not generated any more, thereby reducing the content of stable free radicals in the burning tobacco tar and eliminating active oxygen free radicals generated by oxidation reaction; the glycyrrhizic acid has sweet taste, can save the using amount of cane sugar in the cigarettes, effectively reduce the tar of the cigarettes, neutralize the alkaloid in the tobaccos and relieve the toxicity of nicotine; the oil and fat components have physical adsorption function, and can adsorb part of tar.
The prepared popping essential oil is brownish red or brown in appearance and has liquorice faint scent, the content of licoflavone in the prepared popping essential oil is not less than 0.2%, the content of glycyrrhizic acid is not less than 0.1%, and the prepared popping essential oil contains high effective components. The grease solvent is caprylic capric acid glyceride or monocaprylic acid glyceride or the mixture ratio of the two, so that the appearance of the bead blasting essential oil is clear and transparent and is more attractive.
Drawings
FIG. 1 is a process flow for preparing exploded bead essential oil.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present disclosure and fall within the scope of the appended claims.
And (3) liquorice extractum: extracting dried Glycyrrhrizae radix with 10, 8, 6 times of 70% ethanol at 80 deg.C for 2 hr, filtering, mixing filtrates, and recovering solvent.
Example 1
Dissolving the licorice extract with 3 times of absolute ethyl alcohol, adding 10% concentrated sulfuric acid with mass fraction equivalent to 1 time of the licorice extract, esterifying for 3h in water bath at 50 ℃, standing, and removing supernatant to obtain an esterification product; and (2) adding water with the mass being 10 times that of the licorice extract into the esterification product, extracting the esterification product by using ethyl acetate with the mass being 10 times that of the licorice extract, standing the mixture for 30min, taking the upper layer, adding a mixture (the mass ratio is 2:1) of caprylic/capric glyceride and glyceryl monocaprylate with the mass being 8 times that of the licorice extract, removing the solvent (ethyl acetate) by using a rotary evaporator, wherein the temperature of the rotary evaporator is 55-75 ℃, adding water with the mass being 0.6 time that of the upper layer extract for 2 times in the process, and spin-drying the water.
The content of licoflavone in the bead blasting essential oil is 0.41%, and the content of glycyrrhizic acid is 0.16%; the appearance is clear and transparent.
Example 2
Dissolving the licorice extract with 5 times of absolute ethyl alcohol, adding 20% concentrated sulfuric acid with mass fraction equivalent to 1 time of the licorice extract, esterifying for 5h in water bath at 40 ℃, standing, and removing supernatant to obtain an esterification product; and (3) adding water with the mass being 8 times that of the raw material licorice extract into the esterification product, dissolving the esterification product in the water, extracting the esterification product by using ethyl acetate with the mass being 6 times that of the raw material licorice extract, standing the mixture for 60min, taking the upper layer, adding caprylic/capric glyceride with the mass being 7 times that of the raw material licorice extract, removing the solvent by using a rotary evaporator, wherein the temperature of the rotary evaporator is 55-75 ℃, adding water with the mass being 0.3 time that of the upper layer extract in the process for 3 times, and spin-drying the water.
The content of licoflavone in the exploded bead essential oil is 0.35%, and the content of glycyrrhizic acid is 0.14%; the appearance is clear and transparent.
Example 3
Dissolving the licorice extract with 4 times of absolute ethyl alcohol, adding 15% concentrated sulfuric acid with mass fraction equivalent to 1 time of the licorice extract, esterifying for 2h in water bath at 60 ℃, standing, and removing supernatant to obtain an esterification product; adding water with the mass being 6 times of that of the raw material licorice extract into the esterification product, dissolving the esterification product in the water, extracting the esterification product by using ethyl acetate with the mass being 4 times of that of the raw material licorice extract, standing the mixture for 40min, taking the upper layer, adding a mixture (the mass ratio is 1:1) of caprylic/capric glyceride and monocaprylic glyceride with the mass being 6 times of that of the raw material licorice extract, removing the solvent by using a rotary evaporator, wherein the temperature of the rotary evaporator is 55-75 ℃, adding water with the mass being 0.5 time of that of the upper layer extract for 2 times in the process, and spin-drying the water.
The content of licoflavone in the exploded bead essential oil is 0.33%, and the content of glycyrrhizic acid is 0.14%; the appearance is clear and transparent.
Example 4
Dissolving the licorice extract with 6 times of absolute ethyl alcohol, adding 10% concentrated sulfuric acid with mass fraction equivalent to 1 time of the licorice extract, esterifying for 3h in 55 ℃ water bath, standing, and removing supernatant to obtain an esterification product; and (3) adding water with the mass 5 times that of the raw material licorice extract into the esterification product, extracting with ethyl acetate with the mass 4 times that of the licorice extract, standing for 30min, taking the upper layer, adding glycerol with the mass 7 times that of the raw material licorice extract, removing the solvent by using a rotary evaporator, wherein the temperature of the rotary evaporator is 55-75 ℃, adding water with the mass 0.6 time that of the upper layer extract for 1 time in the process, and spin-drying the water.
The content of licoflavone in the exploded bead essential oil is 0.16%, and the content of glycyrrhizic acid is 0.04%; the appearance was hazy.
Example 5
Dissolving the licorice extract with 9 times of absolute ethyl alcohol, adding 20% concentrated sulfuric acid with mass fraction equivalent to 1 time of the licorice extract, esterifying for 4h in 45 ℃ water bath, standing, and removing supernatant to obtain an esterification product; and (3) adding water with the mass being 6 times that of the raw material licorice extract into the esterification product, dissolving the esterification product in the water, extracting the esterification product by using ethyl acetate with the mass being 5 times that of the raw material licorice extract, standing the mixture for 50min, taking the upper layer, adding propylene glycol with the mass being 6 times that of the raw material licorice extract, removing the solvent by using a rotary evaporator, wherein the temperature of the rotary evaporator is 55-75 ℃, adding water with the mass being 0.2 time that of the upper layer extract in the process for 3 times, and spin-drying the water.
The content of licoflavone in the bead blasting essential oil is 0.10%, and the content of glycyrrhizic acid is 0.06%; the appearance was hazy.
Example 6
Dissolving the licorice extract with 7 times of water, extracting with 6 times of ethyl acetate, standing for 45min, taking the upper layer, adding a mixture of caprylic/capric glyceride and monocaprylic glyceride (mass ratio of 1:1) which is 8 times of the raw material licorice extract, removing the solvent by using a rotary evaporator, adding water which is 0.5 times of the upper layer extract for 2 times during the process, and spin-drying the water.
The content of licoflavone in the bead blasting essential oil is 0.19%, and the content of glycyrrhizic acid is 0.05%; the appearance is clear and transparent.
And (3) measuring the content of licoflavone:
preparation of control solution 10mg of liquiritin control was weighed precisely and placed in a 10ml measuring flask, methanol was added to a constant volume, and shaken well to obtain a liquiritin solution of 1 mg/ml.
Preparation of standard curve A standard curve is drawn by precisely sucking 20, 40, 60, 80, 100 and 120 mul of liquiritin reference substance solution, respectively adding 1ml of methanol, then adding 1ml of 10% KOH solution, standing for 5min, diluting to 10ml with methanol, carrying out blank, measuring absorbance at 334nm, and drawing with absorbance as ordinate and reference substance concentration as abscissa.
The determination method comprises precisely sucking 100 μ l of test sample solution, adding 1ml of methanol, adding 1ml of 10% KOH solution, standing for 5min, diluting with methanol to 10ml, detecting absorbance at 334nm, and calculating licoflavone content.
The product contains licoflavone not less than 0.2% calculated on anhydrous substance.
And (3) glycyrrhizic acid content determination:
octadecylsilane chemically bonded silica is used as a filler in chromatographic conditions and system adaptability experiments; acetonitrile is taken as a mobile phase A, 0.08 percent phosphoric acid is taken as a mobile phase B, and elution is carried out according to the following gradient; the detection wavelength was 252 nm. The theoretical plate number is not less than 5000 calculated according to glycyrrhizic acid peak.
Preparation of control solution A proper amount of glycyrrhizic acid control was precisely weighed and added with 95% ethanol to obtain 0.3mg/ml glycyrrhizic acid solution.
Preparation of the standard curve 1, 2, 4, 8 and 10ml of standard application liquid are precisely absorbed and respectively placed in 10ml volumetric flasks, and the volume of distilled water is constant. A standard curve was plotted with the concentration (mg/ml) as the abscissa and the peak area as the ordinate. The preparation of the test solution is carried out by precisely measuring 1ml of the product, diluting with 80% acetonitrile and fixing the volume to 50ml to obtain the test solution. The determination method comprises precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and determining according to the above chromatographic conditions.
The content of glycyrrhizic acid in the product is not less than 0.1% calculated on anhydrous substance.
Claims (4)
1. The preparation method of the pearl blasting essential oil is characterized by comprising the following steps: taking the licorice extract to carry out esterification reaction; extracting the esterification product with ethyl acetate, mixing the upper layer extract with a grease solvent, and removing the extraction solvent to obtain exploded bead essential oil;
the esterification reaction method comprises the following steps: dissolving the licorice extract with alcohol, adding concentrated sulfuric acid, reacting for 2-5 h at 30-60 ℃, and removing supernatant to obtain an esterification product;
the esterification reaction solvent is absolute ethyl alcohol with the mass 2-5 times that of the licorice extract, the mass fraction of concentrated sulfuric acid is 5-20%, and the adding amount of the concentrated sulfuric acid is 1-2 times that of the licorice extract;
dissolving the esterification product with 6-10 times of water by mass of the licorice extract, and adding 4-10 times of ethyl acetate by mass of the licorice extract for extraction;
the grease solvent is glyceryl monocaprylate and glyceryl caprylate/caprate;
the grease solvent is prepared by mixing glyceryl monocaprylate and glyceryl caprylate caprate according to the ratio of 0-2: 1, and the adding amount of the grease solvent is 6-8 times of the mass of the licorice extract.
2. The popping essential oil prepared by the preparation method of claim 1.
3. Use of the beading essential oil according to claim 2 for the manufacture of a beading cigarette holder.
4. A bead blasting cigarette holder, characterized in that the bead blasting essential oil of claim 2 is used.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107550771A (en) * | 2017-06-29 | 2018-01-09 | 湖南大三湘油茶生态产业有限公司 | Salubrious camellia makeup remover of quality and preparation method thereof |
| CN108060014A (en) * | 2017-12-12 | 2018-05-22 | 湖北中烟工业有限责任公司 | For the preparation method of the Flos Caryophylli extract of quick-fried pearl base oil |
| CN108285830A (en) * | 2018-01-24 | 2018-07-17 | 云南中烟工业有限责任公司 | A kind of cigarette quick-fried pearl herbal essential oil and quick-fried pearl preparation method |
| CN109022151A (en) * | 2018-07-13 | 2018-12-18 | 江苏浩丰生物科技有限公司 | A kind of cigarette of Siraitia grosvenorii flavor quick-fried pearl liquid and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200808333A (en) * | 2006-04-17 | 2008-02-16 | Kaneka Corp | Licorice polyphenol preparation |
| IT1402923B1 (en) * | 2010-12-10 | 2013-09-27 | Rode Pharma S R L | EXTRACTION METHOD OF ACTIVE MOLECULES FROM NATURAL RESINS AND THEIR USE |
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- 2019-04-29 CN CN201910354505.0A patent/CN110079393B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107550771A (en) * | 2017-06-29 | 2018-01-09 | 湖南大三湘油茶生态产业有限公司 | Salubrious camellia makeup remover of quality and preparation method thereof |
| CN108060014A (en) * | 2017-12-12 | 2018-05-22 | 湖北中烟工业有限责任公司 | For the preparation method of the Flos Caryophylli extract of quick-fried pearl base oil |
| CN108285830A (en) * | 2018-01-24 | 2018-07-17 | 云南中烟工业有限责任公司 | A kind of cigarette quick-fried pearl herbal essential oil and quick-fried pearl preparation method |
| CN109022151A (en) * | 2018-07-13 | 2018-12-18 | 江苏浩丰生物科技有限公司 | A kind of cigarette of Siraitia grosvenorii flavor quick-fried pearl liquid and preparation method thereof |
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