CN111747846A - Comprehensive utilization method of star anise - Google Patents

Comprehensive utilization method of star anise Download PDF

Info

Publication number
CN111747846A
CN111747846A CN202010616935.8A CN202010616935A CN111747846A CN 111747846 A CN111747846 A CN 111747846A CN 202010616935 A CN202010616935 A CN 202010616935A CN 111747846 A CN111747846 A CN 111747846A
Authority
CN
China
Prior art keywords
illicium verum
dregs
volatile oil
star anise
extracting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010616935.8A
Other languages
Chinese (zh)
Inventor
罗金花
刘琳琪
赵晨曦
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changsha University
Original Assignee
Changsha University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changsha University filed Critical Changsha University
Priority to CN202010616935.8A priority Critical patent/CN111747846A/en
Publication of CN111747846A publication Critical patent/CN111747846A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07GCOMPOUNDS OF UNKNOWN CONSTITUTION
    • C07G99/00Subject matter not provided for in other groups of this subclass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention relates to a comprehensive utilization method of star anise. The method comprises the following steps: s1, adding water into the illicium verum powder, soaking for 15-18h according to the material-liquid ratio of 1g:8-16mL, and then extracting by adopting a steam distillation method to obtain volatile oil, an extracting solution and illicium verum dregs; s2, carrying out rotary evaporation and concentration on the extracting solution to obtain shikimic acid; s3, distilling the illicium verum dregs obtained in the step S1 with ethanol, and then adding water into the treated illicium verum dregs to perform ultrasonic treatment under the ultrasonic power of 240-; or extracting the illicium verum dregs obtained in the step S1 by ethanol reflux to obtain flavone. Volatile oil, shikimic acid, polysaccharide and flavone are comprehensively extracted from the illicium verum powder, so that the comprehensive utilization of the illicium verum is realized.

Description

Comprehensive utilization method of star anise
Technical Field
The invention relates to the field of extraction of star anise, in particular to a comprehensive utilization method of star anise.
Background
The star anise is a fruit of a plant of the genus illicium of the family illicaceae and has a wide range of edible and medicinal values. The prior art has more researches on the star anise, and various substances such as shikimic acid or volatile oil and the like are extracted from the star anise, but the problem of low utilization rate of the star anise generally exists.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: how to realize the comprehensive utilization of the star anise.
In order to solve the technical problems, the invention provides a comprehensive utilization method of star anise.
A comprehensive utilization method of star anise comprises the following steps:
s1, adding water into the illicium verum powder, soaking for 15-18h according to the material-liquid ratio of 1g:8-16mL, and then extracting by adopting a steam distillation method to obtain volatile oil, an extracting solution and illicium verum dregs;
s2, carrying out rotary evaporation and concentration on the extracting solution to obtain shikimic acid;
s3, distilling the illicium verum dregs obtained in the step S1 with ethanol, and then adding water into the treated illicium verum dregs to perform ultrasonic treatment under the ultrasonic power of 240-; or reflux-extracting the illicium verum dregs obtained in the step S1 by adopting ethanol to obtain the flavone.
Further, in step S1, the star anise powder is obtained by sieving the ground star anise through a 20-100 mesh sieve.
Further, in step S1, extracting for 1.5-4h by the steam distillation method to obtain the volatile oil, the extracting solution and the illicium verum dregs.
Further, in step S3, the illicium verum dregs obtained in step S1 are extracted by reflux with 60-70% ethanol by volume concentration to obtain flavone.
Further, in step S3, the illicium verum dregs obtained in step S1 are extracted by ethanol under reflux for 2-3h to obtain flavone.
Further, in step S3, the illicium verum dregs obtained in step S1 are extracted by ethanol under reflux at 75-80 ℃ for 2-3h to obtain flavone.
Further, in step S3, adding water into the treated Illicium verum dregs according to the feed-liquid ratio of 1g:10-20mL, and performing ultrasonic treatment at the ultrasonic power of 240-.
Further, in step S3, adding water into the treated Illicium verum dregs according to the feed-liquid ratio of 1g:10-20mL, and performing ultrasonic treatment at the ultrasonic power of 240-.
Compared with the prior art, the invention has the advantages that: soaking the illicium verum powder in water according to a feed liquid ratio of 1g:8-16mL for 15-18h, then extracting volatile oil, an extracting solution and illicium verum dregs by a steam distillation method, primarily obtaining volatile oil from the illicium verum, in the distillation process, feeding shikimic acid of the illicium verum into the extracting solution, then carrying out rotary evaporation and concentration on the extracting solution to obtain shikimic acid, wherein low-molecular sugar can greatly influence the extraction of polysaccharide, distilling the illicium verum dregs by ethanol to remove the low-molecular sugar in the illicium verum dregs, then adding water into the treated illiverum dregs for ultrasonic treatment under an ultrasonic power of 240 and 400W to obtain polysaccharide, further extracting the dregs by using the medicine on the basis of extracting the volatile oil to obtain polysaccharide, or extracting the illicium verum dregs by ethanol reflux to obtain flavone, the method provided by the invention comprehensively extracts the volatile oil, shikimic acid, polysaccharide and flavone from the illicium verum powder, thereby realizing the comprehensive utilization of the illicium verum; wherein the extraction rate of the volatile oil is as high as 10.48 percent; the extraction rate of polysaccharide is as high as 7.31%; the extraction rate of the total flavone is as high as 17.67 percent; the extraction rate of shikimic acid is also 2.02%.
Drawings
The features and advantages of the present invention will be more clearly understood by reference to the accompanying drawings, which are illustrative and not to be construed as limiting the invention in any way, in which:
FIG. 1 is a graph showing the effect of particle size of Illicium verum powder on the extraction rate of volatile oil in an embodiment of the present invention.
FIG. 2 is a graph showing the effect of the feed liquid ratio of Illicium verum powder and water on the extraction rate of volatile oil in the embodiment of the present invention.
FIG. 3 is a graph showing the effect of extraction time ratio on the extraction rate of volatile oil in the embodiment of the present invention.
FIG. 4 is a graph of a standard polysaccharide curve obtained in accordance with an embodiment of the present invention.
Fig. 5 is a graph of rutin standard curve obtained in the embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of other modifications without departing from the spirit and scope thereof as defined by the appended claims.
The specific embodiment provides a comprehensive utilization method of star anise, which comprises the following steps:
s1, adding water into the illicium verum powder, soaking for 15-18h according to the material-liquid ratio of 1g:8-16mL, and then extracting for 1.5-4h by adopting a steam distillation method to obtain volatile oil, an extracting solution and illicium verum dregs; the star anise powder is obtained by sieving the ground star anise by 20-100 meshes;
s2, carrying out rotary evaporation and concentration on the extracting solution to obtain shikimic acid;
s3, distilling the illicium verum dregs obtained in the step S1 with ethanol, and then adding water into the treated illicium verum dregs according to the feed-liquid ratio of 1g:10-20mL, and carrying out ultrasonic treatment at the ultrasonic power of 240-400W for 20-40min to obtain polysaccharide; or reflux-extracting the Illicium verum dregs obtained in step S1 with 60-70% ethanol at 75-80 deg.C for 2-3h to obtain flavone.
The study procedure of the present invention is described in detail below:
1 optimal process of star anise volatile oil
(1) Pretreatment of star anise
Crushing the purchased aniseed processed product, respectively sieving the crushed aniseed processed product with 20 meshes, 40 meshes, 60 meshes, 80 meshes and 100 meshes of sieve, packaging the aniseed processed product with a thin plastic bag, and storing the aniseed processed product to a dry place for later use.
(2) Research on single factor of star anise volatile oil
According to a method for measuring volatile oil in XD (appendix XD of 2015 edition of Chinese pharmacopoeia), a special volatile oil extractor is used for extracting volatile oil under the following conditions, and the extracted volatile oil is bottled, numbered, sealed and refrigerated in a refrigerator for later use.
Particle size: taking 5 parts of star anise, sieving 20g of each part of star anise respectively by 20 meshes, 40 meshes, 60 meshes, 80 meshes and 100 meshes, adding 200mL of distilled water into each part of star anise, soaking for 15h, and calculating the oil yield of the star anise respectively, wherein the extraction time is 2 h.
Material-liquid ratio: taking 5 parts of star anise, each part of the star anise is 20g, sieving the star anise with a 40-mesh sieve, adding 160mL, 200mL, 240mL, 280mL and 320mL of distilled water respectively, soaking the star anise for 15 hours, and calculating the oil yield of the star anise respectively, wherein the extraction time is 2 hours.
Extracting time: taking 5 parts of star anise, each part is 20g, sieving by a 40-mesh sieve, adding 200mL of distilled water into each part, soaking for 15h, and respectively calculating the oil yield of 1.5h, 2h, 2.5h, 3h and 3.5 h.
(3) Orthogonal experiment search optimum extraction process
According to factors influencing the extraction of the volatile oil, on the basis of a single-factor experiment, the granularity (A), the material-liquid ratio (B) and the extraction time (C) are selected as investigation factors, each factor is designed to have 3 levels, and the oil yield (%) of the volatile oil is taken as an investigation index to design L9 (3)3) Orthogonal experiments, factor levels are shown in table 1.
TABLE 1 levels of Experimental factors
Figure BDA0002564106140000051
1.1 Single factor experiment
Extracting volatile oil of fructus Anisi Stellati to obtain the influence of granularity on the extraction rate of volatile oil, as shown in FIG. 1; the influence of feed liquid ratio on the extraction rate of volatile oil is shown in FIG. 2; and the effect of extraction time on the extraction rate of volatile oil, as shown in fig. 3.
1.2 orthogonal experiments
From the results of the orthogonal experiment, R was found by analysis as shown in Table 2C>RA>RB>RDThe comprehensive oil yield is taken as an index, and the influence of each factor is C>A>B>D. From the analysis of variance, as shown in Table 2, it can be seen that B has a significant effect (P)<0.05), A and C, namely the feed-liquid ratio is a main factor influencing the oil yield of the star anise, and the extraction time and the granularity influence but have no significance on the oil yield. Combining the analysis of K value of each factor, the measurement result table 2 of the comprehensive orthogonal experiment and the variance analysis table 3, A3B3C2D3The extraction method is a better extraction condition for extracting the star anise volatile oil by a steam distillation method, namely, the star anise volatile oil is sieved by a 60-mesh sieve, the material-liquid ratio is 1:14, the extraction time is 2.5 hours, and the yield of the star anise volatile oil is as high as 10.48 percent.
TABLE 2L 9 (3)3) Results of orthogonal experiments and measurements
Figure BDA0002564106140000061
TABLE 3 ANOVA TABLE
Figure BDA0002564106140000062
Figure BDA0002564106140000071
2 extraction of Illicium verum shikimic acid
And (3) adopting a steam distillation method, sieving by using an optimal extraction process for 60 meshes, wherein the material-liquid ratio is 1:14, extracting for 2.5 hours, and extracting the volatile oil in the star anise. After the volatile oil is extracted, the extract in the bottle is subjected to rotary evaporation and concentration, the methanol constant volume is determined, the shikimic acid content in the extract is measured, and the shikimic acid yield is calculated. Three experiments show that the yield of shikimic acid is 2.02 percent on average.
Optimal process for polysaccharide in illicium verum dregs
(1) Distilling the Illicium verum dregs with the highest volatile oil yield for 2h with absolute ethanol solution, filtering with distilled water, and drying in an oven.
(2) 2g of dried illicium verum dregs are weighed, the polysaccharide in the dregs is extracted by an ultrasonic extraction method, the material-liquid ratio, the ultrasonic power and the ultrasonic time are selected as investigation factors, orthogonal experiments are designed, and the experimental conditions are shown in table 4.
TABLE 4 levels of Experimental factors
Figure BDA0002564106140000072
3.1 method for measuring the content of total polysaccharides in the Illicium verum dregs
(1) Drawing of polysaccharide standard curve
The content of the polysaccharide can be determined by a phenol-sulfuric acid method, firstly, preparing a standard glucose solution with the concentration of 0.2mg/mL, sequentially measuring the standard glucose solutions of 0, 0.2, 0.4, 0.6, 0.8 and 1.0mL, respectively putting the standard glucose solutions into different volumetric flasks, numbering the solutions, and then using distilled water to fix the volume of the volumetric flask containing the glucose solution to 2.0 mL. And 1mL of 5% phenol, 5mL of concentrated H were added2SO4At this time, the solution heated to orange color, after about 30min, it was cooled, and at this time, the absorbance of the solution was measured by spectrophotometry, and the first solution was used as a control, the wavelength was adjusted to 490 nm, and the absorbance of the solution was measured, and the average value was taken 3 times. Finally, the glucose concentration was calculated from the obtained data, and a standard curve of the polysaccharide was prepared with the glucose concentration (x) as abscissa and the absorbance (y) corresponding to each group of solutions as ordinate, as shown in fig. 4.
(2) Determination of the Total polysaccharide content
Extracting polysaccharide under the optimal conditions in orthogonal experiment, measuring absorbance of the obtained polysaccharide solution by the above phenol-sulfuric acid method, and comparing the polysaccharide standard curve with the absorbance to calculate polysaccharide concentration. The polysaccharide extraction rate under such conditions can be obtained by the following formula (1) for the total polysaccharide extraction rate.
Figure BDA0002564106140000081
3.2 Anise Stellati dregs polysaccharide extraction orthogonal experiment
From table 5, it can be derived: under three factors influencing the extraction rate of the polysaccharides, the factor influencing the extraction rate of the polysaccharides is the power of ultrasound, the ratio of a sample to distilled water is followed, the time of ultrasound influencing the extraction rate is the minimum, and the optimal extraction conditions of the aniseed polysaccharides are further obtained as the feed-liquid ratio of 1: 20. the ultrasonic power is 400W, and the ultrasonic time is 20 min.
TABLE 5L 9 (3)3) Polysaccharide orthogonal experiment and determination results
Figure BDA0002564106140000091
3.3 measurement of Total polysaccharide content in the dregs of Illicium verum L
3.3.1 drawing of polysaccharide Standard Curve
Polysaccharide standard curve, as shown in figure 4.
3.3.2 determination of the content of Total polysaccharides of Illicium verum
And (3) combining the polysaccharide standard curve with the formula (1) of the extraction rate of the total polysaccharides to obtain the content of the total polysaccharides in the illicium verum dregs of decoction of 7.31 percent.
Figure BDA0002564106140000101
4 extraction of flavone from Illicium verum dregs
(1) Filtering the illicium verum dregs with the highest volatile oil yield by using gauze, and drying in an oven at 70 ℃ for later use.
(2) Weighing 2g of medicine residue powder in a round-bottom flask, and performing reflux extraction by using 70% ethanol, wherein the material-liquid ratio is 1: 40, refluxing time 2h, extraction temperature 80 ℃.
4.1 measurement of Total Flavonoids in Illicium verum dregs
(1) Drawing of rutin standard curve
Preparing a rutin standard substance into a solution with the concentration of 0.1840mg/mL, accurately transferring 0mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL and 2.5mL into a 10mL volumetric flask, and respectively adding absolute ethyl alcohol to 5 mL; respectively adding 0.3mL of 5% sodium nitrite solution, and reacting for 6 min; respectively adding 0.3mL of 10% aluminum nitrate solution, and reacting for 6 min; then 4mL of 4% sodium hydroxide solution is added respectively, the volume is determined immediately by absolute ethyl alcohol, and the reaction is carried out for 15 min. And (3) determining the absorbance value at the wavelength of 500nm by taking the first bottle of solution as a blank control, measuring for 3 times, taking an average value, taking the absorbance value as a vertical coordinate, and taking the concentration of the rutin control solution as a horizontal coordinate, and obtaining a curve in the form of y ═ ax + b. y is absorbance, and x is rutin standard solution concentration (mg/mL).
(3) Determination of Total Flavonoids content
Taking 0.5mL of flavone extracted from the illicium verum dregs in a 10mL volumetric flask, and adding absolute ethyl alcohol to a constant volume. 1.00mL of the sample was accurately taken out of the flask, transferred to a 10mL volumetric flask, and the absorbance at a wavelength of 500nm was measured with reference to the conditions for drawing a rutin standard curve. And (3) calculating the content of the total flavone in the illicium verum dregs by using the rutin standard curve and the formula (2) of the extraction rate of the total flavone, and measuring for 3 times to obtain an average value.
Figure BDA0002564106140000111
4.2 drawing of rutin Standard Curve
The rutin concentration and absorbance value are plotted to obtain a rutin standard curve, as shown in figure 5.
4.3 determination of Total Flavonoids content in Illicium verum
And (3) combining the rutin standard curve and the formula (2) of the extraction rate of the total flavonoids to obtain the content of the total flavonoids in the illicium verum dregs.
Figure BDA0002564106140000112
5 GC-MS analysis of the component of the volatile oil of star anise
(1) GC-MS analysis conditions
The gas chromatography conditions comprise quartz capillary column (30mm × 0.25.25 mm × 0.25.25 μm) with model number of HP-5MS, and programmed temperature conditions of initial temperature of 60 deg.C and temperature of 3 deg.C/min-1At a rate of 150 ℃ at 10 ℃ min-1The rate of (2) is increased to 200 ℃ and kept for 1 min; sample introduction amount: 1 mu L of the solution; sample inlet temperature: 250 ℃; carrier gas: 99.999% helium; carrier gas flow rate 20 mL/min-1(ii) a The split ratio is 40: 1; the solvent is delayed for 3 min.
The GC-MS results show that: the essential components of the star anise volatile oil are o-cymene, 4-terpene alcohol, 4-allyl anisole, anethole, alpha-pinene, 2, 6-dimethyl-6- (4-methyl-3-pentenyl) bicyclo [3.1.1] hept-2-ene, 1-caryophyllene, 2, 6-dimethyl-6- (4-methyl-3-pentenyl) bicyclo [3.1.1] hept-2-ene, caryophyllene, cis-beta-farnesene, isoeugenol methyl ether and S- (Z) -3,7, 11-trimethyl-1, 6, 10-dodecanetrien-3-ol.
6 determination of antioxidant activity of star anise volatile oil
(1) First, about 0.02600g of DPPH was accurately weighed out in a dark place, and dissolved in 100mL of absolute ethanol to obtain a desired DPPH/ethanol solution, which was then placed in a cool-dry dark place.
(2) Accurately measuring 0.0512g, 0.0755g, 0.989g, 0.1244g and 0.1523g of the anise volatile oil, respectively placing the anise volatile oil, the 0.1244g and the 0.1523g of the anise volatile oil into a clean 25mL volumetric flask, then fixing the volume by using prepared ethanol to obtain the anise volatile oil solution with the required concentration gradient, numbering and sealing in a cool and dry place.
(3) When the antioxidant activity of the substances needs to be measured, dark reaction is carried out on the prepared DPPH-ethanol solution and the prepared star anise volatile oil solution according to the proportioning condition shown in the table 6, after the dark reaction is carried out for about 30min, the dark reaction and the prepared star anise volatile oil solution are subjected to spectrophotometric measurement, the wavelength is adjusted to be 517nm, the absorbance of the fading solution is measured for 3 times respectively, and the average value is obtained.
(4) After the absorbance data is obtained, statistics and induction are carried out, and the DPPH-free radical clearance rate of the star anise volatile oil, namely the antioxidant activity of the volatile oil, is calculated according to a formula (3).
Clearance (%) [ 1- (Ai-Aj)/a 0] × 100% (3)
TABLE 6 DPPH method test sample adding table
Figure BDA0002564106140000121
The removal of DPPH free radicals was determined for solutions of Illicium verum volatile oil at different concentrations, and the results of antioxidant activity of the volatile oil were obtained, as shown in Table 7.
TABLE 7 results of antioxidant Activity of essential oils
Figure BDA0002564106140000131
Other beneficial effects are as follows:
(1) the volatile oil in the star anise is extracted by a steam distillation method, the optimal extraction condition is that the granularity is 60 meshes, the material-liquid ratio is 1:14, the extraction time is 2.5h, and the yield of the star anise volatile oil is up to 10.48 percent. After the volatile oil is extracted, the extract in the bottle is concentrated by rotary evaporation, the volume of methanol is constant, and the yield of shikimic acid is 2.02%.
(2) The GC-MS combined method for analyzing the components of the volatile oil of the star anise shows that: respectively o-cymene, 4-terpene alcohol, 4-allyl anisole, anethole, alpha-pinene, 2, 6-dimethyl-6- (4-methyl-3-pentenyl) bicyclo [3.1.1] hept-2-ene, 1-caryophyllene, 2, 6-dimethyl-6- (4-methyl-3-pentenyl) bicyclo [3.1.1] hept-2-ene, caryophyllene, cis-B-farnesene, isoeugenol methyl ether, S- (Z) -3,7, 11-trimethyl-1, 6, 10-dodecanetrien-3-ol. The research result provides a certain reference basis for the future formulation of the quality management of the fingerprint spectrum of the chemical components of the volatile oil of the illicium verum.
(3) The polysaccharide in the illicium verum dregs is extracted by ultrasonic, and the optimal extraction conditions are that the material-liquid ratio is 1: 20, the ultrasonic power is 400W, and the extraction time is 20 min. The polysaccharide in the aniseed herb residue is extracted by ultrasonic, and the extraction rate is 7.31 percent.
(4) Reflux-extracting with 70% ethanol, wherein the ratio of material to liquid is 1: 40, refluxing for 2h, and extracting the total flavone in the illicium verum dregs at the extraction temperature of 80 ℃, wherein the extraction rate is 17.67 percent.
(5) The volatile oil of the star anise with the mass concentration of 2mg/mL-6mg/mL has a linear relation with DPPH and clearance rate of self-radical. The star anise volatile oil has certain antioxidant capacity.
(6) The research result increases the utilization rate of the active ingredients of the star anise, reduces the use and loss of the raw materials, reduces the cost, and lays a foundation for fully developing the active ingredients of the star anise. The invention provides scientific basis for developing and utilizing the medicinal value of the star anise and the maximum utilization of resources.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The technical features of the embodiments described above can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.

Claims (8)

1. A comprehensive utilization method of star anise is characterized by comprising the following steps:
s1, adding water into the illicium verum powder, soaking for 15-18h according to the material-liquid ratio of 1g:8-16mL, and then extracting by adopting a steam distillation method to obtain volatile oil, an extracting solution and illicium verum dregs;
s2, carrying out rotary evaporation and concentration on the extracting solution to obtain shikimic acid;
s3, distilling the illicium verum dregs obtained in the step S1 with ethanol, and then adding water into the treated illicium verum dregs to perform ultrasonic treatment under the ultrasonic power of 240-; or extracting the illicium verum dregs obtained in the step S1 by ethanol reflux to obtain flavone.
2. The method of claim 1, wherein in step S1, the star anise powder is obtained by sieving the ground star anise through a 20 to 100 mesh sieve.
3. The method of claim 1, wherein in step S1, the volatile oil, the extractive solution, and the illicium verum residue are obtained by steam distillation for 1.5-4 h.
4. The method of claim 1, wherein in step S3, the Illicium verum dregs obtained in step S1 are extracted with 60-70% ethanol by volume concentration under reflux to obtain flavone.
5. The method of claim 1, wherein in step S3, the Illicium verum dregs obtained in step S1 are extracted with ethanol under reflux for 2-3h to obtain flavone.
6. The method of claim 5, wherein in step S3, the Illicium verum dregs obtained in step S1 are extracted with ethanol at 75-80 deg.C under reflux for 2-3h to obtain flavone.
7. The method as claimed in claim 1, wherein in step S3, the treated fructus Anisi Stellati residue is added with water according to a feed-liquid ratio of 1g:10-20mL, and subjected to ultrasonic treatment at an ultrasonic power of 240-400W to obtain the polysaccharide.
8. The method as claimed in claim 7, wherein in step S3, the treated fructus Anisi Stellati residue is added with water according to a feed-liquid ratio of 1g:10-20mL, and subjected to ultrasonic treatment at an ultrasonic power of 240-400W for 20-40min to obtain the polysaccharide.
CN202010616935.8A 2020-07-01 2020-07-01 Comprehensive utilization method of star anise Pending CN111747846A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010616935.8A CN111747846A (en) 2020-07-01 2020-07-01 Comprehensive utilization method of star anise

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010616935.8A CN111747846A (en) 2020-07-01 2020-07-01 Comprehensive utilization method of star anise

Publications (1)

Publication Number Publication Date
CN111747846A true CN111747846A (en) 2020-10-09

Family

ID=72678388

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010616935.8A Pending CN111747846A (en) 2020-07-01 2020-07-01 Comprehensive utilization method of star anise

Country Status (1)

Country Link
CN (1) CN111747846A (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105713732A (en) * 2016-04-29 2016-06-29 山东农业大学 Extraction method of star anise oil

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105713732A (en) * 2016-04-29 2016-06-29 山东农业大学 Extraction method of star anise oil

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
李健等: "八角茴香中精油和莽草酸提取工艺优化", 《食品科学》 *
邹修文等: "八角叶多糖的最佳提取工艺研究", 《化工技术与开发》 *

Similar Documents

Publication Publication Date Title
CN109833377B (en) Camellia oleifera Abel extract and preparation method and application thereof
CN105738546B (en) Method for establishing fingerprint of radix curcumae medicinal material and fingerprint thereof
Piantino et al. Supercritical CO2 extraction of phenolic compounds from Baccharis dracunculifolia
CN102488819B (en) Preparing method for daylily flower extract
Ma et al. Quality evaluation of the rare medicinal plant Dendrobium officinale based on volatile constituents, methanol extracts and polysaccharides
CN106668235A (en) Seedless roxburgh rose general flavone, as well as preparation method and application thereof
CN103705647A (en) Process method for extracting general flavone of golden camellia leaves by CO2 supercritical method
CN107121507B (en) A kind of bamboo shoot shell polyphenol substance measuring method
CN111747846A (en) Comprehensive utilization method of star anise
CN104523820A (en) Low-temperature dynamic extraction process of sophora alopecuroide alkaloid extract
CN101871924B (en) Method for synchronous detection of xanthohumol, isoxanthohumol and 8-isopentenylnaringenin in lupulus
CN112147251B (en) UPC2-PDA-Q-Tof/MS detection method for 42 effective components in schisandra wine
CN101904947A (en) Fructus viticis extract and supercritical preparation process thereof
CN112147249B (en) UPC2-PDA-Q-Tof/MS detection method for 31 effective components in waxberry wine
CN110672744B (en) UPLC fingerprint construction method and detection method of bellyache pills
CN113759012B (en) Quality control method of dianthus superbus formula granules
CN114796331A (en) Method for preparing total flavonoids of fructus aurantii
CN115032287A (en) Quantitative analysis method of tetrahydrocannabinol and cannabidiol
CN103385950B (en) A kind of preparation method of Fructus Rosae Laevigatae total flavones
CN106063828A (en) A kind of oil extracting method of Paeonia suffruticosa blade polyphenol
Li et al. Extraction of aucubin from seeds of Eucommia ulmoides Oliv. using supercritical carbon dioxide
CN115851377B (en) Extraction method for improving quality of Pterocarpus marsupium essential oil and application
CN113087752B (en) Flavone glycoside with antioxidant activity and preparation method and application thereof
CN105381030B (en) Preparation method of trigonelline crude extract
CN115813967B (en) Preparation method of total saponins of adventitious roots of ginseng

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20201009