CN107397838A - A kind of camellia fruit pico-ampere god's perfume (or spice) and preparation method thereof - Google Patents

A kind of camellia fruit pico-ampere god's perfume (or spice) and preparation method thereof Download PDF

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CN107397838A
CN107397838A CN201710763417.7A CN201710763417A CN107397838A CN 107397838 A CN107397838 A CN 107397838A CN 201710763417 A CN201710763417 A CN 201710763417A CN 107397838 A CN107397838 A CN 107397838A
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extract
camellia
pericarp
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extraction
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黄妹兰
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Guangxi Napo County Forestry Science And Technology Park Co Ltd Cui Line
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Guangxi Napo County Forestry Science And Technology Park Co Ltd Cui Line
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    • A61K36/18—Magnoliophyta (angiosperms)
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    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/42—Proteins; Polypeptides; Degradation products thereof; Derivatives thereof, e.g. albumin, gelatin or zein
    • A—HUMAN NECESSITIES
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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
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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    • C11B9/00—Essential oils; Perfumes
    • C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
    • 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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Abstract

The present invention relates to fragrant processing technique field of calming the nerves, more particularly to a kind of camellia fruit pico-ampere god's perfume (or spice) and preparation method thereof, the application prepares perfume (or spice) of calming the nerves using camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract, gelatin and glycerine as raw material, in formula, camellia pericarp extract can play a part of calming the nerves, sterilize, sleeping when burning；Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract can be effectively improved the fragrance for perfume of calming the nerves, and more efficiently facilitate sleep；For willow leaf extract in addition to it can utilize improving fragrance and sleep, bigcatkin willow glucoside therein can also play certain anthelmintic action.The application also uses supercritical CO2Extraction, organic matter solvent extraction and gel separation extraction camellia berry extract；Camellia fruit, which is handled, using microwave and ultrasound pretreatment, which can effectively carry out breaking-wall cell, can effectively ensure the precipitation efficiency of essential oil, polyphenol and flavones.

Description

A kind of camellia fruit pico-ampere god's perfume (or spice) and preparation method thereof
【Technical field】
The present invention relates to fragrant processing technique field of calming the nerves, more particularly to a kind of camellia fruit pico-ampere god's perfume (or spice) and preparation method thereof.
【Background technology】
Camellia pericarp refers to the shell of tea seed, is the accessory substance after the processed utilization of camellia fruit, contains a large amount of essential oils, more The compositions such as contracting pentose, tannin, lignin.The utilization to camellia pericarp is also more and more at present, for example, camellia pericarp can be utilized The separation of polyphenol prepares and anti-oxidant researchs and produces the products such as tannin extract, furancarboxylic acid, activated carbon.Pentosan in camellia pericarp is through water Xie Houke generates furfural, and chaff can only extract from agricultural byproducts, be widely used in the industries such as oil, chemical industry, medicine, agricultural chemicals.But There is presently no the research extracted on camellia fruit peel essential oil, because camellia pericarp impurity is more, shell thickness is not easy to carry out Pretreatment, and it is also immature using area research to camellia fruit peel essential oil, but contain abundant essential oil in camellia pericarp Composition, if can be used, it will greatly improve the deep processing ability of camellia pericarp；, will not and camellia essential oil taste is light Human body is damaged, calmed the nerves perfume (or spice) available for preparation.
【The content of the invention】
In view of the above, it is necessary to which camellia fruit essential oil can be extracted by providing one kind, greatly improve the deep processing of camellia pericarp Ability, for preparing the incense prescription and preparation method thereof of calming the nerves for perfume of calming the nerves.
To reach above-mentioned purpose, the technical solution adopted in the present invention is：
A kind of camellia fruit pico-ampere god is fragrant, and the perfume (or spice) of calming the nerves comprises the following components in parts by weight：23 parts -36 parts of camellia fruit Bark extract, 9 parts -15 parts of Herba Lysimachiae foenumgraeci extract, 10 parts -17 parts of Flos Bombacis Malabarici extract, the extraction of 16 parts -24 parts of Folium Pterocaryae Thing, 13 parts -25 parts of gelatin and 12 parts -24 parts of glycerine.
Further, the camellia pericarp extract extracting method comprises the following steps：
(1) Microwave Pretreatment：The drying camellia pericarp for taking moisture content to be 2%-6%, which is ground into, can pass through the mesh sieve of 50 mesh -70 The powder of net；Then put the powder into and Microwave Extraction is carried out in Microwave Extraction device, complete Microwave Pretreatment process；It is described micro- The frequency of ripple processing is 2560MHZ, power 1000W, processing time 40min；
(2) ultrasound pretreatment：It is 75% by the camellia pericarp powder after step (1) Microwave Pretreatment and percentage by volume (v/v) ethanol is 1 according to mass ratio:3-5 ratio mixing；It is then placed in supersonic extractors and is ultrasonically treated；It is described It is 300w/L-400w/L to be ultrasonically treated ultrasonic power density；It is 150 DEG C -170 DEG C to be ultrasonically treated temperature；Be ultrasonically treated it is total when A length of 50min；
(3) refluxing extraction：Camellia pericarp powder after supersound process is put into refluxing extraction tank with alcohol mixture Row refluxing extraction 4h filtration dryings obtain camellia pericarp crude extract to moisture for 5%；
(4) extract：The crude extract of step (3) is divided into etc. two parts of quality, then a copy of it is put into extraction kettle Carry out CO2Supercritical extract, obtain camellia pericarp extract I；Another carries out gel separation after organic matter solvent extraction Obtain camellia pericarp extract II and camellia pericarp extract III；
(5) mix：By camellia pericarp extract I, camellia pericarp extract II and camellia pericarp extract III according to quality Than for 1-3:2-4:1.
Further, the flow of step (4) supercritical extract is 53L/min, extracting pressure 60MPa, and extraction is warm Spend for 60 DEG C, 55 DEG C of resolution temperature, extraction time 5h.
Further, the solvent-extracted extracting process of step (4) organic matter is：By the crude extract of step (3) according to Mass ratio is 1:Crude extract and water are mixed to get mix suspending thing by 2-3 ratio, are then added and the equal matter of mix suspending thing Measure the petroleum ether extraction of ratio and stand petroleum ether extract after 4h-5h, then fling to the petroleum ether of residual, then add equal The ethyl acetate of mass ratio, stand 4h-5h；The method of gel separation is：By the ethyl acetate extract layer after standing 4h-5h The silicagel column for being put into the mesh of 300 mesh -400 carries out chromatographic isolation；Collect through chloroform-methanol system gradient elution, then again through hydroxypropyl Base sephadex column purifies to obtain camellia pericarp extract II；Through the isolated camellia pericarp extract of reverse silica gel column chromatography Ⅲ；
Further, step (4) the chloroform-methanol system is 10-15 according to mass ratio by chloroform and methanol:1 composition.
The application also provides a kind of fragrant its preparation method of camellia fruit pico-ampere god, and this method comprises the following steps：
(1) each material composition is weighed by above-mentioned parts by weight, then will be put into 100 DEG C of water-bath after gelatin heating fusing Row water bath with thermostatic control, obtains gelatin solution；By camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract It is put into mixer and is stirred with glycerine mixing, speed of agitator 2000r/min-3000r/min, mixing time 30min- 40min obtains emulsion；
(2) NaOH solution for being 1% with mass concentration and with the HCl solution that mass concentration is 1% by step (1) emulsion The pH value of regulation is 7-8；
(3) step (2) is regulated and be sufficiently stirred in the gelatin of the emulsion addition water bath with thermostatic control of pH value, it is uniformly mixed Conjunction is cooled to after room temperature mixture being put into 2 DEG C -3 DEG C of refrigerating box and refrigerated, cold preservation time 12h-14h.
The present invention has the advantages that：
1st, the application uses camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract, bright Glue and glycerine prepare perfume (or spice) of calming the nerves as raw material, and in formula, abundant camellia fruit essential oil, more is can extract out in camellia pericarp extract Phenol and flavones, it can play a part of calming the nerves when burning, sterilize, sleeping, but camellia fruit essential oil taste is light, will not stimulate human body Nerve, if sleeping effect will be greatly improved by adding some Rose Absolutes, applicant has found that addition smokes clothing by lot of experiments Careless extract, Flos Bombacis Malabarici extract, willow leaf extract can be effectively improved the fragrance for perfume of calming the nerves, and more efficiently facilitate sleep；Willow For leaf extract in addition to it can utilize improving fragrance and sleep, bigcatkin willow glucoside therein can also play certain anthelmintic action, can more promote Enter sleep；And the glycerine in applying can promote scattered, the mediation of each extract；Gelatin can be condensed each material.
2nd, the application uses supercritical CO2Extraction, organic matter solvent extraction and gel separation extraction camellia fruit carry Take thing；Supercritical CO2Extraction extraction essential oil is simple to operate, ripe, and recovery rate is high, the high impurity of purity is few；Due to camellia Fruit pericarp thickness is not easy to pre-process, if to extract essential oil will largely effect on the output capacity of essential oil, the application without pretreatment Microwave and ultrasound pretreatment processing is carried out to camellia fruit can effectively carry out breaking-wall cell, be follow-up CO2Extraction, organic matter are molten Agent extraction and gel separation are prepared and can effectively ensure the precipitation efficiency of essential oil, polyphenol and flavones.
【Embodiment】
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification (including any accessory claim, summary), unless specifically stated otherwise, each Feature is an example in a series of equivalent or similar characteristics.
Embodiment 1：
A kind of camellia fruit pico-ampere god's perfume (or spice) of the present embodiment comprises the following components in parts by weight：23 parts of camellia pericarp extraction Thing, 9 parts of Herba Lysimachiae foenumgraeci extract, 10 parts of Flos Bombacis Malabarici extract, 16 parts of willow leaf extract, 13 parts of gelatin and 12 parts Glycerine.
Above-mentioned camellia pericarp extract extracting method comprises the following steps：
(1) Microwave Pretreatment：The drying camellia pericarp for taking moisture content to be 2% is ground into the powder that can pass through 50 eye mesh screens； Then put the powder into and Microwave Extraction is carried out in Microwave Extraction device, complete Microwave Pretreatment process；The microwave treatment Frequency is 2560MHZ, power 1000W, processing time 40min；
(2) ultrasound pretreatment：It is 75% by the camellia pericarp powder after step (1) Microwave Pretreatment and percentage by volume (v/v) ethanol is 1 according to mass ratio:3 ratio mixing；It is then placed in supersonic extractors and is ultrasonically treated；It is described super Sonication ultrasonic power density is 300w/L；It is 150 DEG C to be ultrasonically treated temperature；The total duration of supersound process is 50min；
(3) refluxing extraction：Camellia pericarp powder after supersound process is put into refluxing extraction tank with alcohol mixture Row refluxing extraction 4h filtration dryings obtain camellia pericarp crude extract to moisture for 5%；
(4) extract：The crude extract of step (3) is divided into etc. two parts of quality, then a copy of it is put into extraction kettle Carry out CO2Supercritical extract, obtain camellia pericarp extract I；Another carries out gel separation after organic matter solvent extraction Obtain camellia pericarp extract II and camellia pericarp extract III；Wherein, the flow of supercritical extract process is 53L/min, extraction Pressure power is 60MPa, and extraction temperature is 60 DEG C, 55 DEG C of resolution temperature, extraction time 5h；Wherein, organic matter is solvent-extracted Extracting process is：By the crude extract of step (3) according to mass ratio be 1:Crude extract is mixed to get to mix by 2-3 ratio with water to be hanged Float, then add with mix suspending thing equal quality than petroleum ether extraction and stand petroleum ether extract after 4h, Ran Houhui Go residual petroleum ether, then add equal quality than ethyl acetate, stand 4h；Wherein, the method for gel separation is：Will Stand the silicagel column progress chromatographic isolation that the ethyl acetate extract layer after 4h is put into 300 mesh；Collect through chloroform-methanol (wherein, chlorine Imitation-carbinol system is 10 according to mass ratio by chloroform and methanol:1 composition) system gradient elution, then again through hydroxypropyl glucan Gel column purifies to obtain camellia pericarp extract II；Through the isolated camellia pericarp extract III of reverse silica gel column chromatography；
(5) mix：By camellia pericarp extract I, camellia pericarp extract II and camellia pericarp extract III according to quality Than for 1:2:1.
The extracting method of the fragrant Herba Lysimachiae foenumgraeci extract of above-mentioned camellia fruit pico-ampere god is：The drying that moisture content is 3% is smoked into clothing The whole strain of grass is screened after crushing by the screen cloth of 100 mesh, obtained lavender powder；Lavender powder addition supersonic cell is broken In broken machine, and the mass ratio of good and sound material-water ratio is 1:4 carry out the sodium chloride solution that mass percent is 3% with lavender powder Mixing, is then 1000w in power；Frequency is 23kHz；Temperature handles 50min under conditions of being 50 DEG C, then puts mixture Enter in steam distillation apparatus and distilled, after steam condensation, take supernatant to obtain Herba Lysimachiae foenumgraeci extract.
The extracting method of the fragrant Flos Bombacis Malabarici extract of above-mentioned camellia fruit pico-ampere god is：By the dry common bombax flower that moisture content is 3% Crush and cross 50 mesh sieves and obtain dry powder, be then 85% ethanol with 1 by common bombax flower dry powder and percentage by volume:4 mass ratio adds Extractor, carries out heating and refluxing extraction 4 hours, extracts 4 times, mixes the extract of 4 extractions, obtain common bombax flower crude extract；Then Common bombax flower crude extract is filtered to get filtrate through 200 eye mesh screens, then by falling film concentration plants be concentrated under reduced pressure by filtrate Flos Bombacis Malabarici extract, in falling film concentration technique, vacuum is -0.04MPa to -0.08MPa, maintains the temperature at 90 DEG C, is concentrated to Concentrate is distilled for 1/4 times of stoste and then through molecular distillation equipment, wherein, the charging rate 3ml/ of molecular distillation equipment min；Vapo(u)rizing temperature is 60 DEG C；It 30 is Pa that the vacuum of molecular distillation, which is,；Obtain Flos Bombacis Malabarici extract.
The extracting method of the fragrant willow leaf extract of above-mentioned camellia fruit pico-ampere god is：Willow of the age of tree more than 2 years will be gathered Leaf is ground, and is then 1 by the mass ratio of solid-liquid ratio:4 add the ethanol solution that percentage by volume is 75%, then will mixing Thing is put into supersonic extractors and extracted, and extraction power is 800w；Frequency is 50kHz；Temperature is handled under conditions of being 60 DEG C 20min, then extracted using refluxing extraction, extraction time 3h, filter to take filtrate and carry out rotary evaporation concentration, drying, Until moisture content obtains Folium Pterocaryae extract for 3%.
The fragrant preparation method of calming the nerves of the present embodiment comprises the following steps：
(1) each material composition is weighed by above-mentioned parts by weight, then will be put into 100 DEG C of water-bath after gelatin heating fusing Row water bath with thermostatic control, obtains gelatin solution；By camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract It is put into mixer and is stirred with glycerine mixing, speed of agitator 2000r/min, mixing time 30min obtains emulsion；
(2) NaOH solution for being 1% with mass concentration and with the HCl solution that mass concentration is 1% by step (1) emulsion The pH value of regulation is 7；
(3) step (2) is regulated and be sufficiently stirred in the gelatin of the emulsion addition water bath with thermostatic control of pH value, it is uniformly mixed Conjunction is cooled to after room temperature mixture being put into 2 DEG C of refrigerating box and refrigerated, cold preservation time 12h.
Embodiment 2：
A kind of camellia fruit pico-ampere god's perfume (or spice) of the present embodiment comprises the following components in parts by weight：36 parts of camellia pericarp extraction Thing, 15 parts of Herba Lysimachiae foenumgraeci extract, 17 parts of Flos Bombacis Malabarici extract, 24 parts of willow leaf extract, 25 parts of gelatin and 24 parts Glycerine.
Above-mentioned camellia pericarp extract extracting method comprises the following steps：
(1) Microwave Pretreatment：The drying camellia pericarp for taking moisture content to be 6% is ground into the powder that can pass through 70 eye mesh screens； Then put the powder into and Microwave Extraction is carried out in Microwave Extraction device, complete Microwave Pretreatment process；The microwave treatment Frequency is 2560MHZ, power 1000W, processing time 40min；
(2) ultrasound pretreatment：It is 75% by the camellia pericarp powder after step (1) Microwave Pretreatment and percentage by volume (v/v) ethanol is 1 according to mass ratio:5 ratio mixing；It is then placed in supersonic extractors and is ultrasonically treated；It is described super Sonication ultrasonic power density is 400w/L；It is 170 DEG C to be ultrasonically treated temperature；The total duration of supersound process is 50min；
(3) refluxing extraction：Camellia pericarp powder after supersound process is put into refluxing extraction tank with alcohol mixture Row refluxing extraction 4h filtration dryings obtain camellia pericarp crude extract to moisture for 5%；
(4) extract：The crude extract of step (3) is divided into etc. two parts of quality, then a copy of it is put into extraction kettle Carry out CO2Supercritical extract, obtain camellia pericarp extract I；Another carries out gel separation after organic matter solvent extraction Obtain camellia pericarp extract II and camellia pericarp extract III；Wherein, the flow of supercritical extract process is 53L/min, extraction Pressure power is 60MPa, and extraction temperature is 60 DEG C, 55 DEG C of resolution temperature, extraction time 5h；Wherein, organic matter is solvent-extracted Extracting process is：By the crude extract of step (3) according to mass ratio be 1:Crude extract and water are mixed to get mix suspending by 3 ratio Thing, then add with mix suspending thing equal quality than petroleum ether extraction and stand petroleum ether extract after 5h, then fling to The petroleum ether of residual, then add equal quality than ethyl acetate, stand 5h；Wherein, the method for gel separation is：Will be quiet Put the silicagel column progress chromatographic isolation that the ethyl acetate extract layer after 5h is put into 400 mesh；Collect through chloroform-methanol (wherein, chlorine Imitation-carbinol system is 15 according to mass ratio by chloroform and methanol:1 composition) system gradient elution, then again through hydroxypropyl glucan Gel column purifies to obtain camellia pericarp extract II；Through the isolated camellia pericarp extract III of reverse silica gel column chromatography；
(5) mix：By camellia pericarp extract I, camellia pericarp extract II and camellia pericarp extract III according to quality Than for 3:4:1.
The extracting method of the fragrant Herba Lysimachiae foenumgraeci extract of above-mentioned camellia fruit pico-ampere god is：The drying that moisture content is 3% is smoked into clothing The whole strain of grass is screened after crushing by the screen cloth of 100 mesh, obtained lavender powder；Lavender powder addition supersonic cell is broken In broken machine, and the mass ratio of good and sound material-water ratio is 1:4 carry out the sodium chloride solution that mass percent is 3% with lavender powder Mixing, is then 1000w in power；Frequency is 23kHz；Temperature handles 50min under conditions of being 50 DEG C, then puts mixture Enter in steam distillation apparatus and distilled, after steam condensation, take supernatant to obtain Herba Lysimachiae foenumgraeci extract.
The extracting method of the fragrant Flos Bombacis Malabarici extract of above-mentioned camellia fruit pico-ampere god is：By the dry common bombax flower that moisture content is 3% Crush and cross 50 mesh sieves and obtain dry powder, be then 85% ethanol with 1 by common bombax flower dry powder and percentage by volume:4 mass ratio adds Extractor, carries out heating and refluxing extraction 4 hours, extracts 4 times, mixes the extract of 4 extractions, obtain common bombax flower crude extract；Then Common bombax flower crude extract is filtered to get filtrate through 200 eye mesh screens, then by falling film concentration plants be concentrated under reduced pressure by filtrate Flos Bombacis Malabarici extract, in falling film concentration technique, vacuum is -0.04MPa to -0.08MPa, maintains the temperature at 90 DEG C, is concentrated to Concentrate is distilled for 1/4 times of stoste and then through molecular distillation equipment, wherein, the charging rate 3ml/ of molecular distillation equipment min；Vapo(u)rizing temperature is 60 DEG C；It 30 is Pa that the vacuum of molecular distillation, which is,；Obtain Flos Bombacis Malabarici extract.
The extracting method of the fragrant willow leaf extract of above-mentioned camellia fruit pico-ampere god is：Willow of the age of tree more than 2 years will be gathered Leaf is ground, and is then 1 by the mass ratio of solid-liquid ratio:4 add the ethanol solution that percentage by volume is 75%, then will mixing Thing is put into supersonic extractors and extracted, and extraction power is 800w；Frequency is 50kHz；Temperature is handled under conditions of being 60 DEG C 20min, then extracted using refluxing extraction, extraction time 3h, filter to take filtrate and carry out rotary evaporation concentration, drying, Until moisture content obtains Folium Pterocaryae extract for 3%.
The fragrant preparation method of calming the nerves of the present embodiment comprises the following steps：
(1) each material composition is weighed by above-mentioned parts by weight, then will be put into 100 DEG C of water-bath after gelatin heating fusing Row water bath with thermostatic control, obtains gelatin solution；By camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract It is put into mixer and is stirred with glycerine mixing, speed of agitator 3000r/min, mixing time 40min obtains emulsion；
(2) NaOH solution for being 1% with mass concentration and with the HCl solution that mass concentration is 1% by step (1) emulsion The pH value of regulation is 8；
(3) step (2) is regulated and be sufficiently stirred in the gelatin of the emulsion addition water bath with thermostatic control of pH value, it is uniformly mixed Conjunction is cooled to after room temperature mixture being put into 3 DEG C of refrigerating box and refrigerated, cold preservation time 14h.
Embodiment 3：
A kind of camellia fruit pico-ampere god's perfume (or spice) of the present embodiment comprises the following components in parts by weight：29 parts of camellia pericarp extraction Thing, 12 parts of Herba Lysimachiae foenumgraeci extract, 13 parts of Flos Bombacis Malabarici extract, 19 parts of willow leaf extract, 19 parts of gelatin and 18 parts Glycerine.
Above-mentioned camellia pericarp extract extracting method comprises the following steps：
(1) Microwave Pretreatment：The drying camellia pericarp for taking moisture content to be 4% is ground into the powder that can pass through 60 eye mesh screens； Then put the powder into and Microwave Extraction is carried out in Microwave Extraction device, complete Microwave Pretreatment process；The microwave treatment Frequency is 2560MHZ, power 1000W, processing time 40min；
(2) ultrasound pretreatment：It is 75% by the camellia pericarp powder after step (1) Microwave Pretreatment and percentage by volume (v/v) ethanol is 1 according to mass ratio:4 ratio mixing；It is then placed in supersonic extractors and is ultrasonically treated；It is described super Sonication ultrasonic power density is 350w/L；It is 160 DEG C to be ultrasonically treated temperature；The total duration of supersound process is 50min；
(3) refluxing extraction：Camellia pericarp powder after supersound process is put into refluxing extraction tank with alcohol mixture Row refluxing extraction 4h filtration dryings obtain camellia pericarp crude extract to moisture for 5%；
(4) extract：The crude extract of step (3) is divided into etc. two parts of quality, then a copy of it is put into extraction kettle Carry out CO2Supercritical extract, obtain camellia pericarp extract I；Another carries out gel separation after organic matter solvent extraction Obtain camellia pericarp extract II and camellia pericarp extract III；Wherein, the flow of supercritical extract process is 53L/min, extraction Pressure power is 60MPa, and extraction temperature is 60 DEG C, 55 DEG C of resolution temperature, extraction time 5h；Wherein, organic matter is solvent-extracted Extracting process is：By the crude extract of step (3) according to mass ratio be 1:Crude extract is mixed to get to mix by 2.5 ratio with water to be hanged Float, then add with mix suspending thing equal quality than petroleum ether extraction and stand petroleum ether extract after 4.5h, then Fling to the petroleum ether of residual, then add equal quality than ethyl acetate, stand 4.5h；Wherein, the method for gel separation For：The silicagel column that ethyl acetate extract layer after standing 4.5h is put into 350 mesh carries out chromatographic isolation；Collect through chloroform-methanol (wherein, chloroform-methanol system is 13 according to mass ratio by chloroform and methanol:1 composition) system gradient elution, then again through hydroxypropyl Base sephadex column purifies to obtain camellia pericarp extract II；Through the isolated camellia pericarp extract of reverse silica gel column chromatography Ⅲ；
(5) mix：By camellia pericarp extract I, camellia pericarp extract II and camellia pericarp extract III according to quality Than for 2:3:1.
The extracting method of the fragrant Herba Lysimachiae foenumgraeci extract of above-mentioned camellia fruit pico-ampere god is：The drying that moisture content is 3% is smoked into clothing The whole strain of grass is screened after crushing by the screen cloth of 100 mesh, obtained lavender powder；Lavender powder addition supersonic cell is broken In broken machine, and the mass ratio of good and sound material-water ratio is 1:4 carry out the sodium chloride solution that mass percent is 3% with lavender powder Mixing, is then 1000w in power；Frequency is 23kHz；Temperature handles 50min under conditions of being 50 DEG C, then puts mixture Enter in steam distillation apparatus and distilled, after steam condensation, take supernatant to obtain Herba Lysimachiae foenumgraeci extract.
The extracting method of the fragrant Flos Bombacis Malabarici extract of above-mentioned camellia fruit pico-ampere god is：By the dry common bombax flower that moisture content is 3% Crush and cross 50 mesh sieves and obtain dry powder, be then 85% ethanol with 1 by common bombax flower dry powder and percentage by volume:4 mass ratio adds Extractor, carries out heating and refluxing extraction 4 hours, extracts 4 times, mixes the extract of 4 extractions, obtain common bombax flower crude extract；Then Common bombax flower crude extract is filtered to get filtrate through 200 eye mesh screens, then by falling film concentration plants be concentrated under reduced pressure by filtrate Flos Bombacis Malabarici extract, in falling film concentration technique, vacuum is -0.04MPa to -0.08MPa, maintains the temperature at 90 DEG C, is concentrated to Concentrate is distilled for 1/4 times of stoste and then through molecular distillation equipment, wherein, the charging rate 3ml/ of molecular distillation equipment min；Vapo(u)rizing temperature is 60 DEG C；It 30 is Pa that the vacuum of molecular distillation, which is,；Obtain Flos Bombacis Malabarici extract.
The extracting method of the fragrant willow leaf extract of above-mentioned camellia fruit pico-ampere god is：Willow of the age of tree more than 2 years will be gathered Leaf is ground, and is then 1 by the mass ratio of solid-liquid ratio:4 add the ethanol solution that percentage by volume is 75%, then will mixing Thing is put into supersonic extractors and extracted, and extraction power is 800w；Frequency is 50kHz；Temperature is handled under conditions of being 60 DEG C 20min, then extracted using refluxing extraction, extraction time 3h, filter to take filtrate and carry out rotary evaporation concentration, drying, Until moisture content obtains Folium Pterocaryae extract for 3%.
The fragrant preparation method of calming the nerves of the present embodiment comprises the following steps：
(1) each material composition is weighed by above-mentioned parts by weight, then will be put into 100 DEG C of water-bath after gelatin heating fusing Row water bath with thermostatic control, obtains gelatin solution；By camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract It is put into mixer and is stirred with glycerine mixing, speed of agitator 2500r/min, mixing time 35min obtains emulsion；
(2) NaOH solution for being 1% with mass concentration and with the HCl solution that mass concentration is 1% by step (1) emulsion The pH value of regulation is 7.5；
(3) step (2) is regulated and be sufficiently stirred in the gelatin of the emulsion addition water bath with thermostatic control of pH value, it is uniformly mixed Conjunction is cooled to after room temperature mixture being put into 2 DEG C of refrigerating box and refrigerated, cold preservation time 13h.
Control group 1：
In camellia fruit pico-ampere god's perfume material that this control group is selected, without using camellia pericarp extract, i.e., by following weight The composition composition of part：9 parts of Herba Lysimachiae foenumgraeci extract, 10 parts of Flos Bombacis Malabarici extract, 16 parts of willow leaf extract, 13 parts bright Glue and 12 parts of glycerine.Other methods are identical with embodiment 1.
Control group 2：
In camellia fruit pico-ampere god's perfume material that this control group is selected, without using Herba Lysimachiae foenumgraeci extract, i.e., by following parts by weight Composition composition：23 parts of camellia pericarp extract, 10 parts of Flos Bombacis Malabarici extract, 16 parts of willow leaf extract, 13 parts Gelatin and 12 parts of glycerine.Other methods are identical with embodiment 1.
Control group 3：
In camellia fruit pico-ampere god's perfume material that this control group is selected, without using Flos Bombacis Malabarici extract, i.e., by following parts by weight Composition composition：23 parts of camellia pericarp extract, 9 parts of Herba Lysimachiae foenumgraeci extract, 16 parts of willow leaf extract, 13 parts bright Glue and 12 parts of glycerine.Other methods are identical with embodiment 1.
Control group 4：
In camellia fruit pico-ampere god's perfume material that this control group is selected, without using willow leaf extract, i.e., by following parts by weight Composition composition：23 parts of camellia pericarp extract, 9 parts of Herba Lysimachiae foenumgraeci extract, 10 parts of Flos Bombacis Malabarici extract, 13 parts bright Glue and 12 parts of glycerine.Other methods are identical with embodiment 1.
Control group 5：
In camellia fruit pico-ampere god's perfume material that this control group is selected, without using glycerine, i.e., by following parts by weight into packet Into：23 parts of camellia pericarp extract, 9 parts of Herba Lysimachiae foenumgraeci extract, 10 parts of Flos Bombacis Malabarici extract, the extraction of 16 parts of Folium Pterocaryae Thing and 13 parts of gelatin.Other methods are identical with embodiment 1.
Control group 6：
Camellia pericarp extract is used only in camellia fruit pico-ampere god's perfume material that this control group is selected, without using other plants Extract component, 23 parts of camellia pericarp extract, 13 parts of gelatin and 12 parts of glycerine.Other methods and embodiment 1 are complete It is identical.
Testing experiment：
Determine embodiment 1-3 and control group 1-6 camellia essential oil, polyphenol, general flavone, kapok essential oil, Lavender, water The content of glucoside is raised, concrete condition is shown in Table 1：
Table 1
As seen from the above table, in camellia pericarp extract there is extractible main component：Camellia essential oil, polyphenol, general flavone；Wood Extractible main component is kapok essential oil in cotton extract；Main component in Herba Lysimachiae foenumgraeci extract is Lavender；Poplar Extractible main component is bigcatkin willow glucoside in willow extract.
Sleep test：
100 body weight, age in days size identical mouse are divided into totally 10 groups of 10/group；It is respectively charged into 5m2Inspection box enter Row observation；Each inspection box provides identical water, food；Test group 1-9 also burns 5g embodiments 1-3 and control group 1- in corner Perfume (or spice) of calming the nerves prepared by 6；And in control group and without using perfume (or spice) of calming the nerves；Test the average length of one's sleep of mouse, observation mouse activity Situation, after testing 15d, extract mouse blood examination whether there is fragrant component residue of calming the nerves, concrete condition is shown in Table 2：
Table 2
As seen from the above table, the length of one's sleep of test example 1-3 fragrant sleep mouse of calming the nerves is more than test example 4-9, is even larger than pair According to group, illustrate that the perfume of calming the nerves of the application has the function that to improve sleep, meanwhile, test example 1-9 and control group are not all detected and calmed the nerves Fragrant component residue, the perfume of calming the nerves for illustrating the application is a kind of safe spices.
In summary, sleep quality can safely and effectively be improved using the method production camellia fruit pico-ampere god perfume (or spice) of the present invention, Play a part of calming the nerves, restoring consciouness.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously Therefore limitation of the scope of the invention can not be interpreted as.It should be pointed out that for the person of ordinary skill of the art, Without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection model of the present invention Enclose.Therefore, protection scope of the present invention should be determined by the appended claims.

Claims (6)

1. a kind of camellia fruit pico-ampere god is fragrant, it is characterised in that the perfume (or spice) of calming the nerves comprises the following components in parts by weight：23 part -36 Part camellia pericarp extract, 9 parts -15 parts of Herba Lysimachiae foenumgraeci extract, 10 parts -17 parts of Flos Bombacis Malabarici extract, 16 parts -24 parts Willow leaf extract, 13 parts -25 parts of gelatin and 12 parts -24 parts of glycerine.
2. a kind of camellia fruit pico-ampere god is fragrant, it is characterised in that the camellia pericarp extract extracting method comprises the following steps：
(1) Microwave Pretreatment：The drying camellia pericarp for taking moisture content to be 2%-6%, which is ground into, can pass through the eye mesh screen of 50 mesh -70 Powder；Then put the powder into and Microwave Extraction is carried out in Microwave Extraction device, complete Microwave Pretreatment process；At the microwave The frequency of reason is 2560MHZ, power 1000W, processing time 40min；
(2) ultrasound pretreatment：It is 75% (v/v) by the camellia pericarp powder after step (1) Microwave Pretreatment and percentage by volume Ethanol according to mass ratio be 1:3-5 ratio mixing；It is then placed in supersonic extractors and is ultrasonically treated；At the ultrasound It is 300w/L-400w/L to manage ultrasonic power density；It is 150 DEG C -170 DEG C to be ultrasonically treated temperature；The total duration of supersound process is 50min；
(3) refluxing extraction：Camellia pericarp powder after supersound process and alcohol mixture are put into refluxing extraction tank and returned Stream extraction 4h filtration dryings obtain camellia pericarp crude extract to moisture for 5%；
(4) extract：The crude extract of step (3) is divided into etc. two parts of quality, then a copy of it is put into extraction kettle and carried out CO2Supercritical extract, obtain camellia pericarp extract I；It is isolated that another carries out gel after organic matter solvent extraction Camellia pericarp extract II and camellia pericarp extract III；
(5) mix：It is according to mass ratio by camellia pericarp extract I, camellia pericarp extract II and camellia pericarp extract III 1-3:2-4:1。
3. a kind of camellia fruit pico-ampere god is fragrant according to claim 2, it is characterised in that step (4) supercritical extract Flow is 53L/min, extracting pressure 60MPa, and extraction temperature is 60 DEG C, 55 DEG C of resolution temperature, extraction time 5h.
4. a kind of camellia fruit pico-ampere god is fragrant according to claim 2, it is characterised in that step (4) the organic matter solvent extraction The extracting process taken is：By the crude extract of step (3) according to mass ratio be 1:Crude extract is mixed to get mixed by 2-3 ratio with water Close suspension, then add with mix suspending thing equal quality than petroleum ether extraction and stand petroleum ether extract after 4h-5h, Then fling to the petroleum ether of residual, then add equal quality than ethyl acetate, stand 4h-5h；The gel separation Method is：The silicagel column that ethyl acetate extract layer after standing 4h-5h is put into the mesh of 300 mesh -400 carries out chromatographic isolation；Collect Through chloroform-methanol system gradient elution, then purify through hydroxypropyl sephadex column to obtain camellia pericarp extract II again；Through The isolated camellia pericarp extract III of reverse silica gel column chromatography.
5. a kind of camellia fruit pico-ampere god is fragrant according to claim 4, it is characterised in that step (4) the chloroform-methanol system According to mass ratio it is 10-15 by chloroform and methanol:1 composition.
6. prepare a kind of fragrant its preparation method of camellia fruit pico-ampere god as claimed in claim 1, it is characterised in that methods described Comprise the following steps：
(1) each material composition is weighed by above-mentioned parts by weight, then will be put into progress perseverance in 100 DEG C of water-bath after gelatin heating fusing Tepidarium, obtain gelatin solution；By camellia pericarp extract, Herba Lysimachiae foenumgraeci extract, Flos Bombacis Malabarici extract, willow leaf extract and sweet Oil mixing, which is put into mixer, to be stirred, speed of agitator 2000r/min-3000r/min, mixing time 30min-40min Obtain emulsion；
(2) NaOH solution for being 1% with mass concentration and with the HCl solution that mass concentration is 1% by step (1) emulsion adjust PH value be 7-8；
(3) step (2) is regulated and be sufficiently stirred in the gelatin of the emulsion addition water bath with thermostatic control of pH value, uniformly mixed cold But refrigerated to mixture being put into 2 DEG C -3 DEG C of refrigerating box after room temperature, cold preservation time 12h-14h.
CN201710763417.7A 2017-08-30 2017-08-30 A kind of camellia fruit pico-ampere god's perfume (or spice) and preparation method thereof Pending CN107397838A (en)

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