CN108126054A - A kind of extracting method of Guangxi Camellia nitidissima general flavone - Google Patents

A kind of extracting method of Guangxi Camellia nitidissima general flavone Download PDF

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CN108126054A
CN108126054A CN201810041888.1A CN201810041888A CN108126054A CN 108126054 A CN108126054 A CN 108126054A CN 201810041888 A CN201810041888 A CN 201810041888A CN 108126054 A CN108126054 A CN 108126054A
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camellia nitidissima
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general flavone
guangxi
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陈俊丞
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Guangxi Tianchang Investment Co Ltd
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K36/82Theaceae (Tea family), e.g. camellia
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    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/10Preparation or pretreatment of starting material
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/37Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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Abstract

The invention belongs to abstraction technique fields, and in particular to a kind of extracting method of Guangxi Camellia nitidissima general flavone.The extracting method of Guangxi Camellia nitidissima general flavone provided by the invention, including carrying out mixing superfine grinding with potassium sulfate powder after golden camellia tea is crushed, it is then added in the extraction kettle of supercritical carbon dioxide extraction apparatus, the temperature and pressure of extraction kettle, separating still is set, extract is collected after extraction from separating still, that is Camellia nitidissima general flavone, and calculate its yield.The present invention using it is micro- cut help and supercritical carbon dioxide extraction method be combined by the way of extract Camellia nitidissima general flavone, technological operation is simple, and extraction efficiency height, no solvent residue, color state is preferable.

Description

A kind of extracting method of Guangxi Camellia nitidissima general flavone
Technical field
The invention belongs to abstraction technique fields, and in particular to a kind of extracting method of Guangxi Camellia nitidissima general flavone.
Background technology
Camellia nitidissima is Theaceae, Camellia, Camellia nitidissima group, Ser. Chrysanthae plant.It is found for the first time in Guangxi in nineteen sixty, and It is formally delivered in nineteen sixty-five, causes the concern of domestic and international plant educational circles and gardening educational circles, especially cause international camellia association Pay much attention to.At home, Camellia nitidissima is known as " tea race queen ", " giant panda of plant kingdom ", is then referred to as " in illusion in foreign countries Yellow camellia ".Guangxi is the center of Camellia nitidissima distribution, thus is known as the native place of Camellia nitidissima, is distributed the ground concentrated the most Area is the anti-city in Guangxi, peaceful, Longzhou, Ningming, Fusui, Sui Zuodeng counties and cities, be secondly Longan, big new, day etc., Wuming, Pingguo With the counties such as Tiandong County.Camellia nitidissima is a kind of very high rare plant of health value, and the floral leaf of Camellia nitidissima can be used as medicine, Ming Dynasty's greatness Medical family's Li Shizhen (1518-1593 A.D.) exists《Compendium of Materia Medica》Middle morning is " camellia tender leaf fry ripe, water is washed in a pan, is edible, can also steam solarization and drink " on the books.Golden flower Tea contains that natural organic germanium, selenium, manganese, vanadium, zinc etc. are a variety of to have human body the micro-, a variety of needed by human of important health-care effect Amino acid, vitamin, tea polyphenols, polysaccharide and flavone compound etc..
It researchs and analyses discovery, has when containing abundant flavonoids when active skull cap components in golden camellia tea and inhibit tumour Growth, anti-aging, cardioprotection and its cell membranes in tissue, enhancement liver metabolism, reduction cholesterol, decompression is antibacterial, enhancing is immune It is the effects that function, civil to be usually used in treating sphagitis, urinary tract infection, hypertension, eliminating greasiness weight-reducing, can be used for improving a poor appetite, It relieves the effect of alcohol and quenches one's thirst.
Contained total flavonoid ingredient is mainly Kaempferol and its glycoside and Quercetin and its glycoside in Camellia nitidissima.Traditional The method of extraction general flavone has hot water extraction method, ethanol extraction method, ultrasonic extraction etc., but these methods all have that time-consuming, The shortcomings such as solvent dosage is big, and extraction efficiency is low, the paper delivered such as Chen Quanbin《Camellia nitidissima oxidation-resistant active ingredient is extracted and its is contained It is fixed to measure》It is middle extracted using boiling water, resin adsorption enrichment and ethanol elution the general flavone in golden camellia tea is extracted, step Cumbersome, general flavone yield is only 2.4%, and the general flavone content in golden camellia tea is 0.72%.
In recent years, for supercritical liquid extraction technique due to relatively low with extraction temperature, mass transfer rate is fast, extraction efficiency height, The features such as no solvent residue, has been used for the extraction and separation of many kinds of substance ingredient, but always yellow about supercritical extract Camellia nitidissima The report of ketone is less, and Chinese patent application CN103705647A discloses a kind of CO2Supercritical methanol technology extracts Camellia nitidissima leaf flavonoids Process, using this method extraction general flavone in organic solvent-free remain, general flavone yield be 3.81%, still, such as What optimizes extractant condition, and it is still a great problem utmostly to improve the yield of Camellia nitidissima general flavone and content.
Invention content
In order to solve the problems in the existing technology, the purpose of the present invention is to provide a kind of Guangxi Camellia nitidissima general flavones Extracting method.The extracting method technological operation of Camellia nitidissima general flavone provided by the invention is simple, and extraction efficiency is high, solvent-free residual It stays, color state is preferable.
The present invention provides a kind of extracting methods of Guangxi Camellia nitidissima general flavone, include the following steps:
S1, it is crushed after Guangxi Camellia nitidissima young leaves is dried, obtains Camellia nitidissima coarse powder, sulfuric acid is added in into above-mentioned Camellia nitidissima coarse powder The weight ratio of potassium powder progress superfine grinding, potassium sulfate powder and Camellia nitidissima coarse powder is 1-5:100,10-20 mesh sieve is crossed, obtains micro- cut Help powder;
S2, micro- cut obtained by step S1 is taken to help powder 80-130g, put into the supercritical carbon dioxide extracting instrument that specification is 1L In extraction kettle, 200-500mL ethyl alcohol is added as entrainer, 1-2h is impregnated, sets extraction kettle temperature as 40-50 DEG C, detach Kettle I temperature is 15-30 DEG C, and separation reactor I I temperature is 40-50 DEG C;
S3, carbon dioxide gas tank valve is opened, sets the flow of carbon dioxide as 15-30L/min, extraction kettle pressure is 15-35MPa, separation reactor I pressure are 10-20MPa, and separation reactor I I pressure is 8-10MPa, when extraction kettle reaches required temperature and pressure After power, extraction, extraction time 2-3h are started the cycle over;
S4, extraction after CO 2 fluid sequentially enter in separation reactor I and separation reactor I I, collect, purify to get.
Further, the weight ratio of potassium sulfate powder and Camellia nitidissima coarse powder is 3 in the step S1:100.
Further, micro- cut obtained by step S1 is taken to help powder 103g in the step S2.
Further, extraction kettle temperature is 50 DEG C in the step S2, and the temperature of separation reactor I is 20 DEG C, separation reactor I I's Temperature is 50 DEG C.
Further, 300mL ethyl alcohol is added in the step S2 as entrainer, ethyl alcohol volumetric concentration is 70-95%.
Further, ethyl alcohol volumetric concentration is 85% in the step S2.
Further, extraction kettle pressure is 25MPa in the step S3, and separation reactor I pressure is 12MPa, and separation reactor I I is pressed Power is 8MPa.
Further, the flow of carbon dioxide is 20L/min, extraction time 2h in the step S3.
The present invention using it is micro- cut help and supercritical carbon dioxide extraction method be combined by the way of extract Camellia nitidissima general flavone, Golden camellia tea by it is micro- cut mode is helped to handle after clasmatosis, cell surface generates fresh section, between auxiliary agent and active ingredient Group or intermolecular mutual absorption or effect occurs, changes its micro-property, specific surface area increase, adsorptivity and polarity increase Add, the dissolubility in supercritical fluid greatly improves, and is conducive to improve extraction yield.Supercritical carbon dioxide extraction method can be with Close to room temperature and CO2It is extracted under gas blanket, effectively prevents the oxidation and loss of heat-sensitive substance, extract and divided From being combined into one, the efficient and energy consumption of extraction is less, reduces expense cost.
Inventor has found that the influence maximum of entrainment agent concentration, pressure and temperature to supercritical extract, and investigate The influence of entrainer volumetric concentration, extraction kettle pressure, separation reactor I pressure, separation reactor I temperature to supercritical extract, obtains four Influence size of a factor to Camellia nitidissima general flavone be:Separation reactor I temperature > entrainer volumetric concentration > separation reactor I pressure > extracts Take kettle pressure;Show that optimum process condition is:Entrainer volumetric concentration be 85%, extraction kettle pressure be 25MPa, separation reactor I temperature It is 20 DEG C to spend, and separation reactor I pressure is 12MPa, and the temperature and pressure of separation reactor I I is respectively 50 DEG C and 8MPa, and extraction time is 2h, the yield of gained general flavone is up to 4.29% under optimum process condition.
Compared with prior art, the technical advantages of the present invention are that:
(1) present invention using it is micro- cut to help be combined with supercritical carbon dioxide extraction method, the extraction of Camellia nitidissima general flavone Efficient, general flavone yield is up to 4.29%.
(2) present invention is using the residual of the Camellia nitidissima general flavone organic solvent-free of supercritical carbon dioxide extraction, color shape State is good, and no alcohol taste can be widely applied to the fields such as health food, drug.
(3) the easy grasp simple for process of extraction Camellia nitidissima general flavone that the present invention uses, production cost are low.
Specific embodiment
The following describes the present invention further through the description of specific embodiments, but this is not the limit to the present invention System, those skilled in the art's basic thought according to the present invention can make various modifications or improvements, but without departing from this The basic thought of invention, is all within the scope of the present invention.
Embodiment 1, a kind of extracting method of Guangxi Camellia nitidissima general flavone
The extracting method of the Guangxi Camellia nitidissima general flavone, includes the following steps:
S1, it is crushed after Guangxi Camellia nitidissima young leaves is dried, obtains Camellia nitidissima coarse powder, sulfuric acid is added in into above-mentioned Camellia nitidissima coarse powder The weight ratio of potassium powder progress superfine grinding, potassium sulfate powder and Camellia nitidissima coarse powder is 1:100,10 mesh sieve is crossed, micro- cut is obtained and helps powder;
S2, micro- cut obtained by step S1 is taken to help powder 101g, put into the extraction for the supercritical carbon dioxide extracting instrument that specification is 1L It taking in kettle, adds ethyl alcohol that 200mL volumetric concentrations are 70% as entrainer, immersion 1h sets extraction kettle temperature as 40 DEG C, Separation reactor I temperature is 15 DEG C, and separation reactor I I temperature is 40 DEG C;
S3, carbon dioxide gas tank valve is opened, sets the flow of carbon dioxide as 15L/min, extraction kettle pressure is 15MPa, separation reactor I pressure are 10MPa, and separation reactor I I pressure is 8MPa, after extraction kettle reaches required temperature and pressure, are started Cycling extraction, extraction time 2h;
S4, extraction after CO 2 fluid enter in separating still, collect, purify to get.
Extracted amount is 18.16g/100g, i.e., recovery rate is 18.16%.
Embodiment 2, a kind of extracting method of Guangxi Camellia nitidissima general flavone
The extracting method of the Guangxi Camellia nitidissima general flavone, includes the following steps:
S1, it is crushed after Guangxi Camellia nitidissima young leaves is dried, obtains Camellia nitidissima coarse powder, sulfuric acid is added in into above-mentioned Camellia nitidissima coarse powder The weight ratio of potassium powder progress superfine grinding, potassium sulfate powder and Camellia nitidissima coarse powder is 3:100,20 mesh sieve is crossed, micro- cut is obtained and helps powder;
S2, micro- cut obtained by step S1 is taken to help powder 103g, put into the extraction for the supercritical carbon dioxide extracting instrument that specification is 1L It taking in kettle, adds ethyl alcohol that 300mL volumetric concentrations are 85% as entrainer, immersion 1h sets extraction kettle temperature as 50 DEG C, Separation reactor I temperature is 20 DEG C, and separation reactor I I temperature is 50 DEG C;
S3, carbon dioxide gas tank valve is opened, sets the flow of carbon dioxide as 20L/min, extraction kettle pressure is 25MPa, separation reactor I pressure are 12MPa, and separation reactor I I pressure is 8MPa, after extraction kettle reaches required temperature and pressure, are started Cycling extraction, extraction time 2h;
S4, extraction after CO 2 fluid enter in separating still, collect, purify to get.
Extracted amount is 21.72g/100g, i.e., recovery rate is 21.72%.
Embodiment 3, a kind of extracting method of Guangxi Camellia nitidissima general flavone
The extracting method of the Guangxi Camellia nitidissima general flavone, includes the following steps:
S1, it is crushed after Guangxi Camellia nitidissima young leaves is dried, obtains Camellia nitidissima coarse powder, sulfuric acid is added in into above-mentioned Camellia nitidissima coarse powder The weight ratio of potassium powder progress superfine grinding, potassium sulfate powder and Camellia nitidissima coarse powder is 5:100,20 mesh sieve is crossed, micro- cut is obtained and helps powder;
S2, micro- cut obtained by step S1 is taken to help powder 105g, put into the extraction for the supercritical carbon dioxide extracting instrument that specification is 1L It taking in kettle, adds ethyl alcohol that 500mL volumetric concentrations are 95% as entrainer, immersion 2h sets extraction kettle temperature as 45 DEG C, Separation reactor I temperature is 30 DEG C, and separation reactor I I temperature is 45 DEG C;
S3, carbon dioxide gas tank valve is opened, sets the flow of carbon dioxide as 20L/min, extraction kettle pressure is 35MPa, separation reactor I pressure are 20MPa, and separation reactor I I pressure is 10MPa, after extraction kettle reaches required temperature and pressure, is opened Beginning cycling extraction, extraction time 3h;
S4, extraction after CO 2 fluid enter in separating still, collect, purify to get.
Extracted amount is 16.65g/100g, i.e., recovery rate is 16.65%.
Comparative example 1, a kind of extracting method of Guangxi Camellia nitidissima general flavone
The extracting method of the Guangxi Camellia nitidissima general flavone is similar to Example 2, as different from Example 2, Camellia nitidissima Coarse powder helps mode to handle without micro- cut, and what is added in supercritical carbon dioxide extracting instrument is 100g Camellia nitidissima coarse powder.
Extracted amount is 12.71g/100g, i.e., recovery rate is 12.71%.
Comparative example 2, a kind of extracting method of Guangxi Camellia nitidissima general flavone
The extracting method of the Guangxi Camellia nitidissima general flavone is similar to Example 2, as different from Example 2, separation reactor I Temperature is 40 DEG C, and separation reactor I I temperature is 30 DEG C.
Extracted amount is 15.48g/100g, i.e., recovery rate is 15.48%.
Comparative example 3, ethanol extraction method
The ethanol extraction method, includes the following steps:
S1, it is crushed after Guangxi Camellia nitidissima young leaves is dried, crosses 10 mesh sieve, obtain Guangxi Gold jasmine tea powder;
S2, Guangxi Gold jasmine tea powder 100g obtained by step S1 is taken, adds in the ethyl alcohol that volumetric concentration is 70%, water-bath reflux carries Take 4h, filter, ethyl alcohol washing, merging filtrate to get.
Extracted amount is 6.62g/100g, i.e., recovery rate is 6.62%.
The yield determination of test example one, Guangxi Camellia nitidissima general flavone
1. test material:The Guangxi Camellia nitidissima that Quercetin, Kaempferol, embodiment 1-3 and comparative example 1-3 are extracted is always yellow Ketone.
2. test method:
Quantitative analysis, chromatographic condition are carried out to Guangxi Camellia nitidissima general flavone by high performance liquid chromatography:
Chromatographic column:Sharpsil-H C18Chromatographic column (5 μm, 4.6 × 250mm);Mobile phase:VMethanol:VWater=70:30;Flow velocity: 1.0mL/min;Detection wavelength:360nm;Column temperature:25℃.
(1) preparation of solution
Standard solution:Compound concentration is the Kaempferol standard solution of the Quercetin of 0.592mg/mL, 0.352mg/mL respectively, Above-mentioned prepared Quercetin standard solution 0.2mL, Kaempferol standard solution 0.6mL are taken, is mixed, is shaken up, obtain containing Quercetin 0.1485mg/mL, Kaempferol 0.2640mg/mL mixed standard solutions.
Testing sample solution:Accurately weigh the Guangxi Camellia nitidissima general flavone that embodiment 1-3 and comparative example 1-2 are obtained by extraction 56.50mg adds 30mL methanol solutions in 100mL three-necked flasks, is heated to reflux 1h, after cooling, with methanol constant volume to 50mL, obtains Testing sample solution.
(2) making of standard curve
It is accurate respectively to measure 1.0,2.0,4.0,8.0,10.0 μ L of mixed standard solution, it injects in high performance liquid chromatograph, Chromatogram is recorded, measures peak area, each solution is surveyed three times, is averaged.It is carried out respectively with respective sample introduction quality and peak area It returns and calculates, obtain standard curve.
(3) measure of general flavone yield
10 μ L of accurate measuring Camellia nitidissima testing sample solution are injected in high performance liquid chromatograph, measure Quercetin, Kaempferol Chromatographic peak area integrated value, the quality of Quercetin, Kaempferol in corresponding sample introduction sample is obtained according to peak area.Using external standard method Calculate Quercetin, Kaempferol percentage composition, through convert Quercetin, Kaempferol percentage composition (%)=sample in quercitrin Quality/11.3 × 100% of element, Kaempferol.
Total flavone glucoside content=(quercetin content+Kaempferol content) × 2.51
General flavone yield=total flavone glucoside content × general flavone extracted amount/golden flower tea powder input amounts
3. result of the test:General flavone yield determination the results are shown in Table 1.
The yield determination result of 1 general flavone of table
Classification Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2 Comparative example 3
Yield/% 4.13 4.29 4.07 2.87 3.82 0.75
Through observation shows that 1-3 of embodiment of the present invention extraction gained general flavones are sepia, no alcohol taste;Comparative example 1 and right The extraction gained general flavone of ratio 2 is yellow, has slightly alcohol taste;The extraction gained general flavone of comparative example 3 is lark, and have strong Alcohol taste, illustrate extraction general flavone it is impure, have dissolvent residual.
As shown in Table 1, the present invention is higher using the general flavone yield that supercritical carbon dioxide extracting golden camellia tea obtains, The general flavone yield highest of middle embodiment 2, the optimised process embodiment for the present invention;Comparative example 1 is compared with Example 2, total yellow Ketone yield has larger difference, illustrates micro- general flavone yield cut and help processing that can improve extraction;Comparative example 2 and 2 phase of embodiment Than general flavone yield has different, illustrates that the temperature of separating still is affected to the extraction yield of general flavone;Comparative example 3 with Embodiment 2 is compared, and general flavone yield is very low, illustrate the present invention it is micro- cut to help be combined extraction with supercritical carbon dioxide extracting mode There are apparent advantages compared with traditional extraction process for the method for Camellia nitidissima general flavone.
The stability of test example two, Guangxi Camellia nitidissima general flavone
1. test material:The Guangxi Camellia nitidissima general flavone that embodiment 1-3 is extracted.
2. test method:
(1) preparation of testing sample solution
The accurate Guangxi Camellia nitidissima general flavone for measuring 10mL embodiments 2 and being obtained by extraction, is put into 100mL volumetric flasks, adds 85% ethyl alcohol constant volume, shakes up.
(2) the sample solution 2mL of above-mentioned preparation is accurately measured, is placed in 25mL volumetric flasks, adds in 50% ethyl alcohol of 10mL, The sodium nitrite solution of 1mL 5% is added, mixing places 6min, adds in the aluminum nitrate solution of 1mL 10%, and mixing is placed 6min adds the sodium hydroxide solution of 10mL 4%, is eventually adding 50% ethyl alcohol constant volume, shakes up.After sample solution colour developing, The determination sample solution absorbance at 510nm wavelength places 150min, and an absorbance is measured every 30min, measures three times, It is averaged.
3. result of the test:Absorbance change amount is shown in Table 2.
2 absorbance measurement result of table
Classification 0/min 30/min 60/min 90/min 120/min 150/min
Embodiment 1 0.312 0.311 0.310 0.298 0.296 0.294
Embodiment 2 0.325 0.324 0.322 0.319 0.315 0.313
Embodiment 3 0.297 0.295 0.294 0.292 0.289 0.286
As shown in Table 2, for the general flavone of embodiment 1-3 extractions in the range of 0-150min, absorbance change is smaller, variation Value is substantially unchanged especially in preceding 60min less than 6%, illustrates that the Camellia nitidissima that extracting method using the present invention obtains is total The stability of flavones is preferable.
Test example three, extracting factor optimization
The many because being known as of efficiency of supercritical CO 2 extraction are influenced, but inventor has found entrainment by a large number of experiments The influence of agent, pressure and temperature to supercritical extract is maximum, and is determined that the principal element for influencing extraction is dense for entrainer volume Degree, extracting pressure, separation reactor I pressure, separation reactor I temperature, and Orthogonal Experiment and Design is carried out, refer to by evaluation of general flavone yield Mark, on the basis of embodiment 2, optimizes the experiment of extractant condition, orthogonal test is referring to table 3.
3 orthogonal test table of table
From the range analysis of table 3 it is found that influence size of four factors to Camellia nitidissima general flavone is:Separation reactor I temperature > Entrainer volumetric concentration > separation reactor I pressure > extraction kettle pressure;Supercritical carbon dioxide can be obtained according to the analysis of the K values of table 3 to carry It takes in the optimised process combinatorial theory of Camellia nitidissima general flavone and is:A3B3C2D1, i.e. entrainer volumetric concentration is 85%, extraction kettle pressure Power is 25MPa, and separation reactor I temperature is 20 DEG C, and separation reactor I pressure is 12MPa, and the temperature and pressure of separation reactor I I is respectively 50 DEG C And 8MPa, extraction time 2h.Present invention gained general flavone yield under optimum process condition is up to 4.29%.
By above-mentioned test example it is found that the embodiment of the present invention 2 is most preferred embodiment, the general flavone yield of embodiment 2 is far high In comparative example 1-3, extraction efficiency height.Meanwhile extracting method using the present invention obtain the color state of Camellia nitidissima general flavone, Stability is preferable, no alcohol taste.

Claims (8)

1. a kind of extracting method of Guangxi Camellia nitidissima general flavone, which is characterized in that include the following steps:
S1, it is crushed after Guangxi Camellia nitidissima young leaves is dried, obtains Camellia nitidissima coarse powder, kalium slfuricum powder is added in into above-mentioned Camellia nitidissima coarse powder The weight ratio of end progress superfine grinding, potassium sulfate powder and Camellia nitidissima coarse powder is 1-5:100,10-20 mesh sieve is crossed, micro- cut is obtained and helps Powder;
S2, micro- cut obtained by step S1 is taken to help powder 80-130g, put into the extraction for the supercritical carbon dioxide extracting instrument that specification is 1L In kettle, 200-500mL ethyl alcohol is added as entrainer, impregnates 1-2h, sets extraction kettle temperature as 40-50 DEG C, separation reactor I temperature It is 15-30 DEG C to spend, and separation reactor I I temperature is 40-50 DEG C;
S3, carbon dioxide gas tank valve is opened, sets the flow of carbon dioxide as 15-30L/min, extraction kettle pressure is 15- 35MPa, separation reactor I pressure are 10-20MPa, and separation reactor I I pressure is 8-10MPa, when extraction kettle reaches required temperature and pressure Afterwards, extraction, extraction time 2-3h are started the cycle over;
S4, extraction after CO 2 fluid sequentially enter in separation reactor I and separation reactor I I, collect, purify to get.
2. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 1, which is characterized in that sulphur in the step S1 The weight ratio of sour potassium powder and Camellia nitidissima coarse powder is 3:100.
3. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 1, which is characterized in that taken in the step S2 Micro- cut obtained by step S1 helps powder 103g.
4. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 1, which is characterized in that extract in the step S2 It is 50 DEG C to take kettle temperature degree, and the temperature of separation reactor I is 20 DEG C, and the temperature of separation reactor I I is 50 DEG C.
5. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 1, which is characterized in that in the step S2 again 300mL ethyl alcohol is added in as entrainer, ethyl alcohol volumetric concentration is 70-95%.
6. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 5, which is characterized in that second in the step S2 Alcohol volume a concentration of 85%.
7. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 1, which is characterized in that extract in the step S3 Kettle pressure is taken as 25MPa, separation reactor I pressure is 12MPa, and separation reactor I I pressure is 8MPa.
8. the extracting method of Guangxi Camellia nitidissima general flavone according to claim 1, which is characterized in that two in the step S3 The flow of carbonoxide is 20L/min, extraction time 2h.
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Application publication date: 20180608