CN110946886A - Tilia flower flavone extract and preparation method and application thereof - Google Patents
Tilia flower flavone extract and preparation method and application thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P37/00—Drugs for immunological or allergic disorders
- A61P37/02—Immunomodulators
- A61P37/04—Immunostimulants
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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Abstract
The invention provides a linden flower flavone extract, a preparation method and an application thereof, wherein the linden flower flavone is extracted by adopting an SBE method, wherein the extraction temperature is 60-90 ℃, the extraction time is 5-15min, the material-liquid ratio is 1-5: 10-30, and the flavone yield is 4-8%; the linden flower flavone is extracted under the optimized process conditions, the extraction yield reaches 6.55% +/-0.27%, and meanwhile, the linden flower flavone is shown to have a certain antibacterial effect. The extraction method provided by the invention not only improves the yield of flavone extraction, but also improves antibacterial activity, reduces production energy consumption, is simple and convenient to operate, is mild in condition, is environment-friendly, and can realize large-scale production.
Description
Technical Field
The invention belongs to the technical field of medical food, and particularly relates to a linden flower flavone extract and a preparation method and application thereof.
Background
Chinese land is large and has various plant varieties, and the compositions of the contained effective components have various characteristics, thereby providing rich resources for the development of the effective plant additive. The effective components of the plants can be extracted and separated by different methods, and the application of the effective components of the plants in different fields is explored, so that the economic value of the effective components of the plants is improved.
Linden is a linden family, linden genus, a group with very obvious characteristics, and is easily distinguished from other groups due to the unique large leaf-shaped bracts on the inflorescence or the infructescence and the common inclined leaves at the base. The tilia amurensis, Tangya and the like divide the world into 25 kinds, wherein 2 kinds of Tilia amurensis, 5 kinds of Europe and 18 kinds of east Asia, 14 kinds of tilia trees, particularly 10 kinds, are naturally distributed in China, and Tilia miqueliana is one of the particularly kinds. According to the reports of the literature, the linden flower has the effects of tonifying qi and stomach, relieving pain and detoxifying, and has the effects of treating and relieving various diseases such as hypertension, heart disease, constipation, insomnia and the like. At present, no report for directly researching chemical components contained in the linden flower exists in China. The research reports of European and American tree species are slightly more, and the research of flavonoid compounds is mainly make internal disorder or usurp. The foreign research make internal disorder or usurp found that the extract of Tilia Miqueliana Maxim flower has been used as anxiolytic for years, and also can be used for treating common cold, bronchitis, etc. because the flavonoid substance can be combined with high affinity benzodiazepine substance, and the benzodiazepine can play immune role by acting with respective receptor. In combination with the existing literature data, no relevant report of the linden flower flavone extract preparation for enhancing immunity and the application research make internal disorder or usurp thereof is found.
The immunity is the ability of the human body to resist external pathogenic factors and maintain the stability of the internal environment, namely the ability of the human immune system to protect itself. The main tasks of immunity are to resist infection of bacteria or viruses, etc., and to maintain normal growth and development and health of life. The reasons why the immune system is unable to exert its protective effect are various. With the acceleration of life rhythm and the enhancement of working pressure of people, mental imbalance, incomplete nutrition, irregular life, incapability of exercising, disordered use of medicines and the like can cause low immunity. The immunity is low, the health of people can be directly influenced, the body disorder affecting daily life, work and study is caused, the immunity is low, and the human body is easy to get ill. In the prior art, the medicine for enhancing the human immunity has the problems of obvious adverse reaction and inaccurate effect.
There are various methods for extracting flavonoids. The traditional water extraction method has the defects that the extracted product contains more impurities such as sugar, protein and the like, so that the high-purity target product is difficult to obtain; the organic solvent extraction method has the problems of large organic solvent residue, high cost, low extraction yield and the like; supercritical fluid extraction is high in energy consumption and is not suitable for large-scale industrial production.
A semi-bionic extraction (SBE) method is a separation technology developed in recent years, and the principle of the SBE method is an extraction process which is designed by simulating the environmental conditions that oral drugs are transported and absorbed through gastrointestinal tracts and sequentially undergoes acid and alkali treatment, so that the category of flavonoids extracted in vitro is more similar to the flavonoid absorbed in vivo through gastrointestinal tract digestion, the biological activity and functions of the flavonoid on organisms can be better explained, the cost is saved, the SBE method is safe and environment-friendly, and people gradually pay attention in recent years. The SBE method is successfully applied to the extraction of flavones such as propolis, folium cortex eucommiae, radix puerariae and the like. In China, related reports of extracting flavones in Chinese toon leaves and radix sophorae flavescentis by adopting an SBE method are provided, but the extraction effect of the SBE method on the flavones in the linden flowers is not reported.
Disclosure of Invention
One of the purposes of the invention is to provide the linden flower flavone extract for enhancing immunity, solve the problems of obvious adverse reaction and uncertain effect of the medicine for enhancing the human immunity in the prior art and promote the comprehensive utilization of the linden flower resource.
In order to achieve the purpose, the invention provides a preparation method and application of a linden flower flavone extract for enhancing immunity.
The preparation method is to extract the tilia flower flavone by an SBE method, and comprises the following steps:
weighing a certain mass of linden flower powder, extracting the linden flower flavone by respectively using disodium hydrogen phosphate-citric acid buffer solutions with the pH values of 2.1-2.3, 7.5-7.8 and 7.9-8.1 as extracting agents, combining filtrates, centrifuging at the rotating speed of 4000-6000r/min for 8-12min, and concentrating the supernatant by using a rotary evaporator to obtain crude extract of the linden flower flavone.
Preferably, the method for extracting the tilia flower flavone by the SBE method comprises the following steps: weighing a certain mass of linden flower powder, extracting the linden flower flavone by using disodium hydrogen phosphate-citric acid buffer solutions with the pH values of 2.2, 7.6 and 8.0 as extracting agents respectively, combining filtrates, centrifuging at the rotating speed of 5000r/min for 10min, taking supernatant, and concentrating by using a rotary evaporator to obtain crude flavone extract.
Preferably, the SBE method in step 1 has the following process parameters: the extraction temperature is 60-90 deg.C, the extraction time is 5-15min, and the material-liquid ratio is 1-5: 10-30.
Preferably, the SBE method in step 1 has the following process parameters: the extraction temperature was 70 ℃.
Preferably, the SBE method in step 1 has the following process parameters: the extraction time is 10min
Preferably, the SBE method in step 1 has the following process parameters: the ratio of the material to the liquid is 1: 20.
The invention can measure the content of the flavonoid compound by the following method:
step 1: drawing a standard curve, measuring the content of the flavonoid compound by adopting a spectrophotometry method taking rutin as a standard substance to obtain a linear regression equation: y ═ ax + b, where: x is the concentration/(mg/mL) of the rutin standard substance; y is absorbance, and a and b are constants obtained by fitting.
Step 2: transferring 1-3mL of the crude flavone extract into a 30-60mL volumetric flask, and adding 3-7% (g/mL) of NaNO31-3mL of the solution is shaken up and kept stand for 4-8 min; adding 5-15% (g/mL) Al (NO)3)31-3mL of the solution is shaken up and kept stand for 3-7 min; adding 15-30mL of 2-6% (g/mL) NaOH solution, shaking, standing for 4-8min, adding distilled water to constant volume, shaking, centrifuging at the rotation speed of 4000-6000r/min for 7-12min, and taking the supernatant to measure the OD value at the position of 450-550 nm; and (3) substituting the measured OD value into the linear regression equation in the step (1) to obtain the flavone content of the crude flavone extracting solution.
And step 3: calculating the extraction rate of the tilia flower flavone, wherein the extraction rate of the tilia flower flavone is CV/(m multiplied by 1000) multiplied by 100 percent; in the formula, C is the flavone content/(mg/mL) of the crude flavone extract; v is the volume/mL of the crude flavone extracting solution; m is the mass/g of the linden flower powder.
Preferably, step 2 comprises the steps of: transferring 1mL of Tilia Miqueliana Maxim flower extract into 50mL volumetric flask, and adding 5% (g/mL) NaNO32mL of the solution is shaken up and kept stand for 6 min; adding 10% (g/mL) Al (NO)3)32mL of the solution is shaken up and kept stand for 6 min; adding 20mL of 4% (g/mL) NaOH solution, shaking, standing for 6min, adding distilled water to desired volume, shaking, centrifuging at 5000r/min for 10min, and collecting supernatant and determining OD value at 510 nm; the extraction rate of the tilia flower flavone is CV/(m multiplied by 1000) multiplied by 100 percent; wherein C is the concentration of flavone in the extract/(mg/mL); v is the volume/mL of the extracting solution; m is the mass/g of the linden flower powder.
The linden flower flavone extract can be used for preparing food, health care products or medicines with the function of enhancing immunity, and the dosage form of the medicines can be capsules, granules, tablets, pills or powder.
Compared with the prior art, the invention has the following beneficial effects:
1. the optimized SBE extraction process parameters are as follows: the extraction temperature is 70 ℃, the extraction time is 10min and the material-liquid ratio is 1: 20 (m: V), the linden flower flavone is extracted under the optimized process conditions, the extraction yield reaches 6.55% +/-0.27%, and meanwhile, the linden flower flavone has a certain antibacterial effect.
2. The SBE method is most advantageous in that the treatment time is short, compared with the ARE method. The test result of the invention shows that the treatment time of the linden flowers is only 10min, which is far less than the heating time of 1.5h experienced by an ARE method; and the extractant replaces organic solvent ethanol with water, so that the SBE method for extracting the flavone substance not only improves the yield, but also improves the antibacterial activity and reduces the production energy consumption.
3. The method is simple and convenient to operate, mild in condition, environment-friendly and capable of realizing large-scale production.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings.
FIG. 1 shows the effect of extraction time on extraction yield.
Figure 2 shows the effect of extraction temperature on extraction yield.
Figure 3 shows the effect of feed-liquid ratio on extraction yield.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
Example 1
The embodiment provides a basswood flower flavone extract and a preparation method thereof.
Step 1: extracting flos Tiliae Miquelianae flavone by SBE method, weighing certain amount of flos Tiliae Miquelianae powder, extracting flos Tiliae Miquelianae flavone with pH of 2.2, 7.6, 8.0 disodium hydrogen phosphate-citric acid buffer solution as extractant, wherein the extraction conditions include: the extraction temperature is 70 deg.C, the extraction time is 10min, and the material-liquid ratio is 1: 20. Mixing filtrates, centrifuging at 5000r/min for 10min, collecting supernatant, and concentrating with rotary evaporator to obtain crude flavone extractive solution.
Step 2: drawing a standard curve, measuring the content of the flavonoid compound by adopting a spectrophotometry method taking rutin as a standard substance to obtain a linear regression equation: y-10.169 x +0.0158, wherein R20.9961, wherein: x is the concentration/(mg/mL) of the rutin standard substance; and y is absorbance.
And step 3: transferring 1mL of Tilia Miqueliana Maxim flower extract into 50mL volumetric flask, and adding 5% (g/mL) NaNO32mL of the solution is shaken up and kept stand for 6 min; adding 10% (g/mL) Al (NO)3)32mL of the solution is shaken up and kept stand for 6 min; adding 20mL of 4% (g/mL) NaOH solution, shaking, standing for 6min, adding distilled water to desired volume, shaking, centrifuging at 5000r/min for 10min, and collecting supernatant and determining OD value at 510 nm; the extraction rate of the tilia flower flavone is CV/(m multiplied by 1000) multiplied by 100 percent; wherein C is the concentration of flavone in the extract/(mg/mL); v is the volume/mL of the extracting solution; m is the mass/g of the linden flower powder.
The extraction yield of the tilia amurensis flowers in the embodiment is 6.55% +/-0.27%.
Example 2
The embodiment provides a basswood flower flavone extract and a preparation method thereof.
Step 1: extracting flos Tiliae Miquelianae flavone by SBE method, weighing certain amount of flos Tiliae Miquelianae powder, extracting flos Tiliae Miquelianae flavone with pH of 2.2, 7.6, 8.0 disodium hydrogen phosphate-citric acid buffer solution as extractant, wherein the extraction conditions include: the extraction temperature is 60 deg.C, the extraction time is 5min, and the material-liquid ratio is 1: 10. Mixing filtrates, centrifuging at 4000r/min for 8-12min, collecting supernatant, and concentrating with rotary evaporator to obtain crude flavone extractive solution.
Step 2: drawing a standard curve, measuring the content of the flavonoid compound by adopting a spectrophotometry method taking rutin as a standard substance to obtain a linear regression equation: y-10.169 x +0.0158, wherein R20.9961, wherein: x is the concentration/(mg/mL) of the rutin standard substance; and y is absorbance.
And step 3: transferring 1mL of Tilia Miqueliana Maxim flower extract into 30mL volumetric flask, and adding 3% (g/mL) of NaNO32mL of the solution is shaken up and kept stand for 4 min; 5% (g/mL) Al (NO) was added3)32mL of the solution is shaken up and kept stand for 3 min; adding 15mL of 2% (g/mL) NaOH solution, shaking up, standing for 4min, adding distilled water to a constant volume, shaking up, centrifuging at a rotating speed of 4000r/min for 7min, and taking the supernatant to measure the OD value at 450 nm; the extraction rate of the tilia flower flavone is CV/(m multiplied by 1000) multiplied by 100 percent; wherein C is the concentration of flavone in the extract/(mg/mL); v is the volume/mL of the extracting solution; m is the mass/g of the linden flower powder.
The extraction yield of the tilia amurensis flowers in the embodiment is 5.56% +/-0.12%.
Example 3
The embodiment provides a basswood flower flavone extract and a preparation method thereof.
Step 1: extracting flos Tiliae Miquelianae flavone by SBE method, weighing certain amount of flos Tiliae Miquelianae powder, extracting flos Tiliae Miquelianae flavone with pH of 2.2, 7.6, 8.0 disodium hydrogen phosphate-citric acid buffer solution as extractant, wherein the extraction conditions include: the extraction temperature is 90 deg.C, the extraction time is 15min, and the material-liquid ratio is 1: 15. Mixing filtrates, centrifuging at 6000r/min for 8-12min, collecting supernatant, and concentrating with rotary evaporator to obtain crude flavone extractive solution.
Step 2: drawing a standard curve, measuring the content of the flavonoid compound by adopting a spectrophotometry method taking rutin as a standard substance to obtain a linear regression equation: y-10.169 x +0.0158, wherein R20.9961, wherein: x is the concentration/(mg/mL) of the rutin standard substance; and y is absorbance.
And step 3: transferring 3mL of linden flower extract into a 60mL volumetric flask, and adding 7% (g/mL) of NaNO3Shaking the solution 3mL evenly, and standing for 8 min; adding 15% (g/mL) Al (NO)3)3Shaking the solution 3mL uniformly, and standing for 7 min; adding 6% (g/mL) NaOH solution 30mL, shaking, standing for 8min, adding distilled water to desired volume, shaking, centrifuging at 6000r/min for 12min, and collecting supernatant and measuring OD value at 550 nm; the extraction rate of the tilia flower flavone is CV/(m multiplied by 1000) multiplied by 100 percent; wherein C is the concentration of flavone in the extract/(mg/mL); v is the volume/mL of the extracting solution; m is the mass/g of the linden flower powder.
The extraction yield of the tilia amurensis flowers in the embodiment is 4.23% +/-0.10%.
Test example
Experimental design for extracting tilia flower flavone by SBE method
The influence of the extraction time on the extraction yield is designed by a single factor experiment: the fixed extraction temperature was 70 deg.C, the feed-to-liquid ratio was 1: 20 (m: V), and the effect of different extraction times (10min, 20min, 30min, 40min and 50min) on the extraction yield was examined.
Influence of extraction temperature on extraction yield: the feed-liquid ratio was fixed at 1: 20 (m: V), extraction was performed for 20min, and the influence of different extraction temperatures (50 deg.C, 60 deg.C, 70 deg.C, 80 deg.C, 90 deg.C) on the extraction yield was examined.
Influence of feed liquid ratio on extraction yield: the fixed extraction temperature was 70 deg.C, the extraction time was 20min, and the effect of different feed-liquid ratios (1: 10 (m: V), 1: 20 (m: V), 1: 30 (m: V), 1: 40 (m: V), 1: 50 (m: V)) on the extraction yield was examined.
The orthogonal experimental design SBE method takes the extraction temperature (A), the extraction time (B) and the feed-liquid ratio (C) as experimental factors, experiments are carried out according to an L9(34) orthogonal table, and the extraction process of the SBE method is optimized.
TABLE 1 orthogonal experiment factor horizon of SBE method
(1) The effect of extraction time on extraction yield is shown in FIG. 1. As can be seen from FIG. 1, the extraction yield increased from 5.05% + -0.07% to 5.83% + -0.12% in the time range of 10-20min, after which the extraction yield decreased with increasing time. Therefore, the optimal extraction time is 20 min.
(2) The effect of extraction temperature on extraction yield is shown in FIG. 2. As can be seen from FIG. 2, in a certain range, the extraction yield of tilia flower flavone tends to increase and decrease with the increase of the extraction temperature, when the temperature is between 60 ℃ and 70 ℃, the extraction yield increases significantly (p is less than 0.01) with the increase of the temperature, when the temperature is higher than 70 ℃, the increase trend of the extraction yield begins to be gentle (p is less than 0.05), and when the temperature is up to 80 ℃, the extraction yield rapidly decreases after reaching the maximum (6.30% +/-0.10%). Therefore, the optimal control of the extraction temperature at 70-80 ℃ is very important in the flavone extraction process.
(3) The effect of feed-liquid ratio on extraction yield is shown in FIG. 3. As can be seen from FIG. 3, the extraction yield of tilia flower flavone increases with the increase of the feed-liquid ratio. When the feed-liquid ratio is 1: 20 (m: V), the extraction yield reaches 6.55% +/-0.23%, and then the extraction yield slowly increases and gradually becomes stable.
From the above experiments, the optimum process parameters of the SBE method are: the extraction temperature is 70 deg.C, the extraction time is 10min, the material-liquid ratio is 1: 20, and the flavone yield is 6.55% +/-0.23%.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (9)
1. A preparation method of a basswood flower flavone extract is characterized in that the preparation method is an SBE method for extracting the basswood flower flavone, and comprises the following steps:
weighing a certain mass of linden flower powder, extracting the linden flower flavone by respectively using disodium hydrogen phosphate-citric acid buffer solutions with the pH values of 2.1-2.3, 7.5-7.8 and 7.9-8.1 as extracting agents, combining filtrates, centrifuging at the rotating speed of 4000-6000r/min for 8-12min, and concentrating the supernatant by using a rotary evaporator to obtain crude extract of the linden flower flavone.
2. The method for preparing a tilia flower flavone extract as claimed in claim 1, comprising the steps of: weighing a certain mass of flos Tiliae Miquelianae powder, extracting flos Tiliae Miquelianae flavone with disodium hydrogen phosphate-citric acid buffer solution with pH of 2.2, 7.6, and 8.0 as extractant, mixing filtrates, centrifuging at 5000r/min for 10min, collecting supernatant, and concentrating with rotary evaporator to obtain crude flavone extractive solution.
3. The method for preparing a tilia flower flavone extract as claimed in claim 1 or 2, wherein the SBE method comprises the following process parameters: the extraction temperature is 60-90 deg.C, the extraction time is 5-15min, and the material-liquid ratio is 1-5: 10-30.
4. The method of preparing a tilia flower flavone extract as set forth in claim 3, wherein the extraction temperature is 70 ℃.
5. The method of preparing a tilia flower flavone extract as claimed in claim 3, wherein the extraction time is 10 min.
6. The method for preparing a tilia flower flavone extract as claimed in claim 3, wherein the ratio of the material to the liquid is 1: 20.
7. A Tilia flavone extract obtained by the method according to any one of claims 1 to 6.
8. The use of the tilia flower flavone extract as set forth in claim 7 for the preparation of foods, health products or medicines having an immunological enhancement effect.
9. The use of claim 8, wherein the medicament is in the form of a capsule, granule, tablet, pill or powder.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104800255A (en) * | 2015-05-11 | 2015-07-29 | 黑龙江中医药大学 | Application of tilia amurensis inflorescence extractive to preparation of medicine for treating insomnia |
| CN106726867A (en) * | 2016-11-17 | 2017-05-31 | 东莞波顿香料有限公司 | A kind of application of the extracting method and the extract of lime tree flower extract |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104800255A (en) * | 2015-05-11 | 2015-07-29 | 黑龙江中医药大学 | Application of tilia amurensis inflorescence extractive to preparation of medicine for treating insomnia |
| CN106726867A (en) * | 2016-11-17 | 2017-05-31 | 东莞波顿香料有限公司 | A kind of application of the extracting method and the extract of lime tree flower extract |
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| 李月娇: "板栗花黄酮的提取、纯化及其生物学功能研究", 《中国优秀硕士学位论文全文数据库 医药卫生科技辑》 * |
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