Method for extracting effective components in poria cocos

Abstract

The invention discloses a method for extracting effective components in poria cocos, which comprises the following steps: taking poria cocos raw powder, adjusting the moisture content of the poria cocos raw powder, then extruding the poria cocos raw powder, keeping the temperature at 30-90 DEG C in the extrusion process, and collecting poria cocos powder after the extrusion is completed; the collected poria cocos powder is crushed, dried and dissolved in a solvent for extraction. According to the method for extracting the effective components in the poria cocos, a traditional method for directly extracting the effective components in the poria cocos by utilizing a solvent is abandoned, the effective components in the poria cocos are innovatively extracted after treatment by adopting a low-temperature extrusion mode before the solvent is added, and cell walls of poria cocos powder are damaged in the extrusion process; the dispersion time of the poria cocos powder in a solvent is shortened, and the extraction yield of effective components such as total polysaccharides, total triterpenes and alcohol-soluble extracts in the poria cocos powder is remarkably improved; extrusion within the temperature range can particularly avoid reduction of total polysaccharide and alcohol-soluble extract components after extraction, and the extraction rate is increased.

Description

Technical Field

[0001] The present application relates to the technical field of extraction of effective ingredients from Poria cocos, and in particular to a method for extracting effective ingredients from Poria cocos. Background Art

[0002] Poria is one of the commonly used clinical medicines. The extract from Poria has the effects of promoting diuresis and eliminating dampness, strengthening the spleen and calming the mind. The existing Poria extraction technology mainly uses direct solvent extraction, and auxiliary enzymes can also be added to extract soluble substances in Poria. This method of operation and extraction is not deep enough, and many effective ingredients in Poria cannot be completely immersed and extracted, and the extraction efficiency of soluble substances is not good. Summary of the invention

[0003] The invention provides a method for extracting effective components from Poria cocos, so as to solve the technical problems in the prior art that many effective components in Poria cocos cannot be extracted and the yield of the effective components is low.

[0004] To achieve the above object, the technical solution provided by the present invention is as follows:

[0005] The invention provides a method for extracting effective ingredients from Poria cocos, comprising the following steps: taking Poria cocos raw powder and adjusting the moisture content thereof, then extruding the powder, maintaining the temperature at 30 DEG C to 90 DEG C during the extrusion process, and collecting Poria cocos blocks after the extrusion is completed; and crushing and drying the collected Poria cocos blocks and dissolving them in a solvent for extraction.

[0006] Furthermore, in the step of taking the Poria cocos powder and adjusting its moisture content, the moisture content of the Poria cocos powder is adjusted to 13% to 50%.

[0007] Furthermore, during the extrusion process, the pressure is maintained at 3 to 10T.

[0008] Furthermore, the extrusion process utilizes a twin-screw extruder for extrusion processing, the feed rate is 1-3 kg / min, and the screw speed is 100-160 r / min.

[0009] Furthermore, the solvent is selected from one or more of water, methanol and ethanol.

[0010] Furthermore, the temperature of drying the Poria cocos block after crushing is 40°C to 60°C.

[0011] Furthermore, the temperature of extracting the Poria cocos block in a solvent after crushing and drying is 30°C to 60°C.

[0012] Furthermore, in the extraction step, the mass volume ratio of the crushed and dried Poria cocos powder to the solvent is 1:15-50 g / mL.

[0013] The extraction method of the effective ingredients in Poria cocos provided by the present invention abandons the traditional method of directly extracting the effective ingredients in Poria cocos by using solvents, and innovatively extracts the effective ingredients in Poria cocos by low-temperature extrusion before adding the solvent. The cell wall of Poria cocos powder is destroyed during the extrusion process, which reduces the dispersion time of Poria cocos powder in the solvent, and significantly improves the extraction yield of effective ingredients such as total polysaccharides, total triterpenes and alcohol-soluble extracts in Poria cocos powder; extrusion within the above temperature range can especially avoid the reduction of total polysaccharides and alcohol-soluble extract components after extraction, and improve the extraction rate. Compared with the un-extruded Poria cocos powder extraction method, the dispersion time of Poria cocos powder after extrusion within the above temperature range is reduced by about 35.27% to 57.17%, and the extraction yields of total polysaccharides, total triterpenes and alcohol-soluble extracts are increased by about 11.45% to 50.03%, 121.24% to 152.30% and 10.85 to 20.61%, respectively. DETAILED DESCRIPTION

[0014] In order to enable those skilled in the art to better understand the technical solutions in this application, the technical solutions in the embodiments of this application will be clearly and completely described below. Obviously, the described embodiments are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0015] The embodiment of the present application provides a method for extracting effective ingredients from Poria cocos, comprising the following steps: taking Poria cocos raw powder and adjusting its moisture content, then extruding it, maintaining the temperature at 30°C to 90°C during the extrusion process, and collecting Poria cocos blocks after the extrusion is completed; crushing and drying the collected Poria cocos blocks and dissolving them in a solvent for extraction.

[0016] Poria cocos, the dried sclerotium of the Polyporaceae fungus Poria cocos (Schw.) Wolf, is a traditional Chinese medicine that is both a food and a medicine. In traditional Chinese medicine, Poria cocos is widely used and is known as "nine out of ten prescriptions contain Poria cocos". Poria cocos is sweet and mild in nature, and has the effects of promoting diuresis and eliminating dampness, strengthening the spleen and stopping diarrhea, and calming the mind. Modern research has also confirmed that it has multiple pharmacological effects such as immunomodulation, anti-tumor, anti-inflammatory, antioxidant, anti-aging, lowering blood sugar and regulating blood lipids. The main components of Poria cocos include polysaccharides and triterpenes, and it also contains trace components such as sterols, proteins, amino acids and inorganic elements.

[0017] Poria powder has poor dispersibility in solvents. In the embodiments of the present application, the cell wall of Poria powder is destroyed after extrusion, the dispersion speed is accelerated, the contact rate between Poria powder and solvent is increased, and the extraction rate of effective ingredients such as total polysaccharides, total triterpenes and alcohol-soluble extracts in Poria powder is improved. Extrusion within the above temperature range can especially avoid the reduction of total polysaccharides and alcohol-soluble extract components and improve their extraction rate.

[0018] The embodiment of the present application abandons the traditional method of directly extracting the effective ingredients in Poria cocos using solvents, and innovatively uses low-temperature extrusion before adding solvents to extract the effective ingredients in Poria cocos. The cell wall of Poria cocos powder is destroyed during the extrusion process, which reduces the dispersion time of Poria cocos powder in the solvent and significantly improves the extraction yield of effective ingredients such as total polysaccharides, total triterpenes and alcohol-soluble extracts in Poria cocos powder; extrusion within the above temperature range can especially avoid the reduction of total polysaccharides and alcohol-soluble extract components after extraction, and improve the extraction rate. Compared with the un-extruded Poria cocos powder extraction method, the dispersion time of Poria cocos powder after extrusion within the above temperature range is reduced by about 35.27% to 57.17%, and the extraction yields of total polysaccharides, total triterpenes and alcohol-soluble extracts are increased by about 11.45% to 50.03%, 121.24% to 152.30% and 10.85 to 20.61%, respectively.

[0019] In the embodiment of the present application, the effective ingredients in Poria cocos are extracted by low-temperature extrusion, and the temperature during the extrusion process is maintained at 30° C. to 90° C. At the above temperature, the reduction of polysaccharides and alcohol-soluble extract components is avoided, and the extraction rate of the effective ingredients in Poria cocos powder can be maximized.

[0020] The extract obtained by the method for extracting the effective ingredients from Poria cocos in the embodiment of the present application has broad application prospects in the fields of health foods, functional beverages, natural food additives, new drug research and development, and formula granules, and can meet the modern people's pursuit of health and quality and promote industrial development.

[0021] In some embodiments, in the step of taking the raw Poria cocos powder and adjusting its moisture content, the moisture content of the raw Poria cocos powder is adjusted to 13% to 50%. In the embodiments of the present application, an appropriate moisture content in the raw Poria cocos powder can improve the fluidity of the raw Poria cocos powder and improve the extrusion effect; if the moisture content is too low, the raw Poria cocos powder is too dry, resulting in poor fluidity; and if the moisture content is too high, it may cause caking and difficulty in extrusion.

[0022] In some embodiments, during the extrusion process, the pressure is maintained at 3 to 10 T. In the embodiments of the present application, when extruding the raw Poria cocos powder, if the pressure is too low, the extrusion effect may be poor; if the pressure is too high, it will not only increase energy consumption, but also cause increased wear of the equipment, or even equipment failure.

[0023] In other embodiments, the extrusion process is performed using a twin-screw extruder, with a feed rate of 1 to 3 kg / min and a screw speed of 100 to 160 r / min.

[0024] In some embodiments, the solvent is selected from one or more of water, methanol, and ethanol. In the embodiments of the present application, the extracts obtained by extraction in different solvents have an effective component with the highest yield. When water is used as the solvent, the total polysaccharide component extraction rate is the highest; when methanol is used as the solvent, the total triterpene component extraction rate is the highest; when ethanol is used as the solvent, the alcohol-soluble extract component extraction rate is the highest.

[0025] In some embodiments, the temperature of drying the tuckahoe block after crushing is 40° C. to 60° C. In the embodiments of the present application, the temperature of drying the tuckahoe powder after crushing is kept within the above range, which can make the water content of the tuckahoe powder less than 8% for easy storage.

[0026] In some embodiments, the extraction temperature of the Poria cocos block in the solvent after crushing and drying is 30° C. to 60° C. In the embodiments of the present application, the extraction temperature in the solvent is maintained within the above range to avoid degradation or destruction of the active ingredients under high temperature conditions.

[0027] In some embodiments, in the extraction step, the mass volume ratio of the crushed and dried Poria powder to the solvent is 1:15-50 g / mL. In the extraction step of the embodiment of the present application, the mass volume ratio of the dried Poria powder to the solvent is ensured to be within the above range, so that the Poria powder can be evenly dispersed in the solvent and the effective ingredients are fully dissolved.

[0028] The present application is described in more detail below with specific examples. All reagents in the following examples are commercially available.

[0029] Example 1

[0030] The method for extracting the active ingredients in Poria cocos comprises the following steps:

[0031] The dried Poria cocos was crushed and the moisture content was adjusted to 30% by spraying water. Then, the dried Poria cocos powder was extruded by a manual tablet press (Changsha Miqi Instrument Equipment Co., Ltd. / MC-12). During the extrusion process, the temperature was maintained at 60°C, the pressure was maintained at 8T, and the extrusion time was 3 minutes. After the extrusion was completed, the Poria cocos pieces were collected. The collected Poria cocos pieces were crushed and dried at 50°C to obtain Poria cocos powder.

[0032] The Poria cocos powder was dissolved in different solvents for extraction, and the dispersion time in different solvents and the contents of main components such as total polysaccharides, total triterpenes and alcohol-soluble extracts were determined.

[0033] Determination method of dispersion time:

[0034] Accurately weigh 1.0 g of the above-mentioned Poria powder sample and place it in 100 mL of a solvent at 50°C. Control the magnetic stirring speed to 500 r / min, and record the time required for the Poria powder to be completely dispersed, which is the dispersion time of the sample in the above-mentioned solvent.

[0035] Extraction method of Poria powder in water:

[0036] Accurately weigh 1.0 g (dry basis) of the Poria cocos sample powder, add 20 mL of distilled water, extract in a 50°C water bath with ultrasonic wave for 2 h, cool to room temperature, centrifuge at 10,000 r / min for 5 min, accurately draw 1 mL of the supernatant, add 4 mL of water, and shake well to obtain the polysaccharide test solution.

[0037] Extraction method of Poria powder in anhydrous methanol:

[0038] Accurately weigh 1.0 g (on a dry basis) of the Poria cocos sample powder, add 20 mL of anhydrous methanol, mix well, perform ultrasonic extraction at 50° C. for 1 h, filter, and dilute to 25 mL to obtain a total triterpene test solution.

[0039] Extraction method of Poria powder in ethanol:

[0040] Accurately weigh 2g of the Poria cocos sample powder, place it in a 100mL conical flask, add 50mL of ethanol, seal it, weigh it, let it stand for 1 hour, connect a reflux condenser, heat it to boiling, and keep it boiling for 1 hour. After cooling, remove the conical flask, seal it, weigh it again, make up the lost weight with ethanol, shake it well, and obtain the alcohol-soluble extract test solution.

[0041] Example 2

[0042] The method for extracting the active ingredients in Poria cocos comprises the following steps:

[0043] The dried Poria cocos was crushed and the moisture content was adjusted to 50% by spraying water. The dried Poria cocos powder was then put into a twin-screw extruder (Shandong Mingben Machinery Co., Ltd. / M32) for extrusion. During the extrusion process, the temperature was maintained at 30°C, the feed rate at the feed port was 1kg / min, and the screw speed was 160r / min. After the extrusion was completed, the Poria cocos pieces were collected. The collected Poria cocos pieces were crushed and dried at 50°C to obtain Poria cocos powder.

[0044] The Poria cocos powder was dissolved in different solvents for extraction, and the dispersion time in different solvents and the contents of main components such as total polysaccharides, total triterpenes and alcohol-soluble extracts were determined.

[0045] The above dispersion method and extraction method are the same as those in Example 1.

[0046] Example 3

[0047] The method for extracting the active ingredients in Poria cocos comprises the following steps:

[0048] The dried Poria cocos was crushed and the moisture content was adjusted to 13% by spraying water. Then, the dried Poria cocos powder was extruded by a manual tablet press (Changsha Miqi Instrument Equipment Co., Ltd. / MC-12). During the extrusion process, the temperature was maintained at 90°C, the pressure was maintained at 5T, and the extrusion time was 3 minutes. After the extrusion was completed, the Poria cocos pieces were collected. The collected Poria cocos pieces were crushed and dried at 60°C to obtain Poria cocos powder.

[0049] The Poria cocos powder was dissolved in different solvents for extraction, and the dispersion time in different solvents and the contents of main components such as total polysaccharides, total triterpenes and alcohol-soluble extracts were determined.

[0050] The above dispersion method and extraction method are the same as those in Example 1.

[0051] Comparative Example 1

[0052] The method for extracting the active ingredients in Poria cocos comprises the following steps:

[0053] Take dried Poria cocos and grind them into powder. Adjust the moisture content to 13% by spraying water and mixing. Pass the powder through a 40-mesh sieve to obtain Poria cocos powder, and set aside.

[0054] The Poria cocos powder was dissolved in different solvents for extraction, and the dispersion time in different solvents and the contents of main components such as total polysaccharides, total triterpenes and alcohol-soluble extracts were determined.

[0055] The above dispersion method and extraction method are the same as those in Example 1.

[0056] Comparative Example 2

[0057] The method for extracting the active ingredients in Poria cocos comprises the following steps:

[0058] The dried Poria cocos was crushed and the moisture content was adjusted to 13% by spraying water. Then, the dried Poria cocos powder was extruded by a manual tablet press (Changsha Miqi Instrument Equipment Co., Ltd. / MC-12). During the extrusion process, the temperature was maintained at 120°C, the pressure was maintained at 3T, and the extrusion time was 3 minutes. After the extrusion was completed, the Poria cocos pieces were collected. The collected Poria cocos pieces were crushed and dried at 50°C to obtain Poria cocos powder.

[0059] The Poria cocos powder was dissolved in different solvents for extraction, and the dispersion time in different solvents and the contents of main components such as total polysaccharides, total triterpenes and alcohol-soluble extracts were determined.

[0060] The above dispersion method and extraction method are the same as those in Example 1.

[0061] The test solutions obtained after extraction with various solvents in Examples 1 to 3 and Comparative Examples 1 and 2 were subjected to determination of effective components. The determination method is as follows:

[0062] Total polysaccharide content determination method:

[0063] 1. Preparation of reference solution: Accurately weigh 10.0 mg of anhydrous glucose reference substance dried to constant weight, dissolve it in distilled water and make up to 100 mL, shake well to obtain 0.1 mg / mL anhydrous glucose reference solution.

[0064] 2. Preparation of standard curve: Accurately measure 0.20mL, 0.40mL, 0.60mL, 0.80mL, 1.00mL and 1.20mL of the above-mentioned reference solution in a reaction tube, add water to 2.0mL each, shake well, accurately add 1.0mL of 5% phenol solution, mix thoroughly, slowly add 6.0mL of concentrated sulfuric acid in an ice water bath, vortex and oscillate for 30s, let stand at room temperature for 30min, and use the corresponding reagent as a blank. According to the UV-Vis spectrophotometry method (General Rule 0401), the absorbance is measured at a wavelength of 490nm. With the absorbance value as the ordinate and the concentration as the abscissa, draw and obtain the standard curve Y=6.0916X+0.0584(R 2 =0.9828).

[0065] 3. The specific determination conditions are as follows: Take 0.2 mL of polysaccharide test solution, measure the absorbance at a wavelength of 490 nm according to the method under the standard curve preparation item, read the content of anhydrous glucose in the test solution from the standard curve, and calculate it.

[0066] Total triterpenoid content determination method:

[0067] 1. Preparation of reference solution: Accurately weigh 10.0 mg of ursolic acid reference substance dried to constant weight, dissolve it in anhydrous methanol and make up to 100 mL, shake well to obtain 0.1 mg / mL ursolic acid reference solution.

[0068] 2. Preparation of standard curve: Accurately measure 0.10mL, 0.20mL, 0.40mL, 0.60mL, 0.80mL and 1.00mL of reference solution in a stoppered graduated test tube, evaporate to dryness, add 0.4mL of 5% vanillin-glacial acetic acid solution and 2.0mL of perchloric acid in turn, mix well and keep warm in a 60℃ constant temperature water bath for 20min, take out, add 5mL of glacial acetic acid after an ice water bath for 10min, mix well, and use the corresponding reagent as blank. According to the UV-Vis spectrophotometry (General Rule 0401), the absorbance is measured at a wavelength of 549nm. With the absorbance value as the ordinate and the volume of the ursolic acid reference substance as the abscissa, draw and obtain the standard curve of Y=0.9564X+0.1397(R 2 =0.9335).

[0069] 3. The specific determination conditions are as follows: Accurately pipette 0.5 mL of total triterpene test solution, measure the absorbance at a wavelength of 549 nm according to the method under the standard curve preparation item, read the volume of ursolic acid in the test solution from the standard curve, and calculate it.

[0070] Determination method of alcohol-soluble extract content:

[0071] The alcohol-soluble extract content of Poria cocos in different examples and comparative examples was determined by the hot leaching method under the alcohol-soluble extract determination method (General Rule 2201). The alcohol-soluble extract test solution was filtered through a drying filter, 25 ml of the filtrate was accurately measured and placed in an evaporating dish that had been dried to constant weight, evaporated to dryness on a water bath, dried at 105°C for 3 hours, cooled in a desiccator for 30 minutes, and the weight was quickly and accurately weighed and the alcohol-soluble extract content (%) in different examples was calculated.

[0072] Through the above-mentioned detection of the Poria extracts in the examples and comparative examples, the dispersion time and the contents of main components such as total polysaccharides, total triterpenes and alcohol-soluble extracts in each sample were obtained, see Table 1.

[0073] Table 1 Dispersion time of Poria powder and content or type of main active ingredients in Examples and Comparative Examples

[0074]

[0075] Note: *P<0.01, VS Example 1; #P<0.01, VS Example 2.

[0076] As for the dispersion time, compared with Comparative Example 1, Example 1, Example 2 and Example 3 can significantly reduce the dispersion time (P<0.01), and compared with Comparative Example 2, Example 1 and Example 2 can significantly increase the dispersion time (P<0.01), indicating that the dispersibility of Poria powder can be improved by high-temperature or low-temperature extrusion, and the higher the extrusion temperature, the shorter the dispersion time. Among them, the dispersion time of Examples 1 to 3 is reduced by 35.27 to 57.17% compared with Comparative Example 1.

[0077] For the total polysaccharide components, compared with Comparative Example 1, Example 1, Example 2 and Example 3 can significantly improve the extraction rate of total polysaccharides (P<0.01); compared with Comparative Example 2, Example 1, Example 2 and Example 3 can significantly improve the extraction rate of total polysaccharides (P<0.01). Comparison of the total polysaccharide extraction rates of Example 1, Example 2 and Example 3 shows that the extraction rate of total polysaccharides in extruded Poria powder first increases and then decreases with the increase of extrusion temperature, among which the total polysaccharide extraction rates of Examples 1 to 3 are increased by 11.45 to 50.03% compared with Comparative Example 1.

[0078] For the total triterpenoid components, compared with Comparative Example 1, Examples 1, 2 and 3 can significantly improve the extraction rate of total triterpenes (P<0.01), but there is no significant difference between different extrusion temperatures, indicating that triterpenoid compounds are relatively stable and insensitive to temperature. However, compared with Comparative Example 1, the extraction rate of total triterpenes in Examples 1 to 3 is still increased by 121.24 to 152.30%.

[0079] For alcohol-soluble extracts, compared with Comparative Example 1, Example 1, Example 2 and Example 3 can significantly improve the extraction yield of the extract (P<0.01); compared with Comparative Example 2, the extraction yield of the extracts of Example 1, Example 2 and Example 3 is also significantly improved (P<0.01). Comparison of the extraction yields of alcohol-soluble extracts of Example 1, Example 2 and Example 3 shows that the extraction yield of alcohol-soluble extracts in extruded Poria powder first increases and then decreases with the increase of extrusion temperature, wherein the extraction yields of alcohol-soluble extracts of Examples 1 to 3 are increased by 10.85 to 20.61% compared with Comparative Example 1.

[0080] Combined with the above experimental results, it can be seen that compared with the embodiment of low-temperature extrusion of Poria cocos powder at 30°C to 90°C, although the dispersion time of the high-temperature extrusion Poria cocos powder group is reduced and the dispersibility is good, the extraction yield of total polysaccharides, total triterpenes and alcohol-soluble extracts is reduced. Therefore, the dispersibility of Poria cocos powder and the extraction yield of total polysaccharides, total triterpenes and alcohol-soluble extracts are comprehensively evaluated, and the selection of Poria cocos powder treated by low-temperature extrusion at 30°C to 90°C is the best choice with a high extraction yield of each active ingredient.

[0081] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for extracting effective ingredients from Poria cocos, characterized in that: The following steps are involved: Taking the original Poria cocos powder and adjusting its moisture content, then extruding it, maintaining the temperature at 30°C to 90°C during the extrusion process, and collecting the Poria cocos blocks after the extrusion is completed; The collected Poria cocos pieces are crushed, dried and dissolved in a solvent for extraction.

2. The method for extracting the active ingredient from Poria cocos according to claim 1, characterized in that: In the step of taking the raw Poria cocos powder and adjusting its water content, the water content of the raw Poria cocos powder is adjusted to 13% to 50%.

3. The method for extracting the effective ingredients from Poria cocos according to claim 1, characterized in that: During the extrusion process, the pressure is maintained at 3-10T.

4. The method for extracting the effective ingredients from Poria cocos according to claim 1, characterized in that: The extrusion process utilizes a twin-screw extruder for extrusion processing, the feed rate is 1-3 kg / min, and the screw speed is 100-160 r / min.

5. The method for extracting the effective ingredients from Poria cocos according to any one of claims 1 to 4, characterized in that: The solvent is selected from one or more of water, methanol and ethanol.

6. The method for extracting the effective ingredients from Poria cocos according to any one of claims 1 to 4, characterized in that: The drying temperature of the tuckahoe block after crushing is 40°C to 60°C.

7. The method for extracting the effective ingredients from Poria cocos according to any one of claims 1 to 4, characterized in that: The temperature of extracting the Poria cocos block in the solvent after it is crushed and dried is 30°C to 60°C.

8. The method for extracting the effective ingredients from Poria cocos according to any one of claims 1 to 4, characterized in that: In the extraction step, the mass volume ratio of the crushed and dried Poria cocos powder to the solvent is 1:15-50 g / mL.

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