Method for comprehensively utilizing poria peel

Abstract

The invention belongs to the field of comprehensive utilization of traditional Chinese medicinal material resources, and discloses a comprehensive utilization method of poria peel. The method can be used for simultaneously producing two products of poria cocos peel formula granules and poria cocos triterpenoid extract by utilizing poria cocos peel, and specifically comprises the following steps: (1) extracting poria cocos peel by adopting a hot water immersion method, filtering, concentrating, drying and granulating to prepare the poria cocos peel formula granules; and (2) extracting the poria cocos peel dregs subjected to hot water extraction by adopting high-concentration alcohol to prepare the poria cocos triterpenoid extract. According to the method, water-soluble components and triterpenoid components in the poria cocos peel medicinal material can be extracted and utilized at the same time, the comprehensive utilization value of the poria cocos peel medicinal material is effectively improved, a new way is provided for treatment of medicine residues after production of the poria cocos peel formula granules, and the additional value of the poria cocos peel is further improved.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of comprehensive utilization of traditional Chinese medicinal material resources, and specifically provides a method for comprehensively utilizing Poria cocos (Schw.) Wolf skin to produce Poria cocos (Schw.) Wolf skin formula granules and Poria cocos (Schw.) Wolf triterpenoid extract. BACKGROUND

[0002] Poria cocos (Schw.) Wolf skin is the outer skin of the dried sclerotium of Poria cocos (Schw.) Wolf in the process of processing, which is brown to black brown in appearance. Poria cocos (Schw.) Wolf triterpenoids are the main pharmacodynamic components in Poria cocos (Schw.) Wolf medicinal materials. Modern pharmacological studies have shown that this kind of components has various significant pharmacological activities such as anti-tumor, anti-inflammatory, anti-oxidation, sedation and hypnotic effect, and thus has attracted widespread attention. Through comparative study on the total content of Poria cocos (Schw.) Wolf triterpenoids in different medicinal parts such as Poria cocos (Schw.) Wolf skin, red Poria cocos (Schw.) Wolf and white Poria cocos (Schw.) Wolf, it is found that the content is in the order of Poria cocos (Schw.) Wolf skin > red Poria cocos (Schw.) Wolf > white Poria cocos (Schw.) Wolf, which shows that the deeper the color of Poria cocos (Schw.) Wolf part, the higher the content of Poria cocos (Schw.) Wolf triterpenoids. Therefore, Poria cocos (Schw.) Wolf skin not only has a lower market price, but also has a higher content of Poria cocos (Schw.) Wolf triterpenoids, and thus has the advantage of being used as the main raw material for extracting Poria cocos (Schw.) Wolf triterpenoids in actual production.

[0003] Traditional Chinese medicine formula granules are a new type of decoction pieces formed by single decoction pieces through water extraction, concentration, drying and granulation. They are safe and effective, accurate in dosage, convenient to take, and meet the development trend of modern society, and thus are increasingly favored by patients. At the same time, how to comprehensively utilize the residues after the production of traditional Chinese medicine formula granules has become an important measure for related enterprises to create a low-carbon economy. In the production process of Poria cocos (Schw.) Wolf skin formula granules, water extraction process is usually used, while Poria cocos (Schw.) Wolf triterpenoids have poor water solubility, which leads to the fact that most of Poria cocos (Schw.) Wolf triterpenoids are left in the residues and finally wasted with the residues; in addition, if the residues are not properly treated, there is a risk of re-entering the market. Therefore, there is an urgent need for a method for comprehensively utilizing Poria cocos (Schw.) Wolf skin to realize the efficient utilization of this traditional Chinese medicinal material resource and create higher economic value, and at the same time avoid the problem of improper circulation of residues. SUMMARY

[0004] In view of this, the present application provides a method for comprehensively utilizing Poria cocos (Schw.) Wolf skin, aiming to solve the problems of waste of triterpenoids and low utilization rate of residues caused by the single production of formula granules from Poria cocos (Schw.) Wolf skin, realize the synchronous production of Poria cocos (Schw.) Wolf skin formula granules and Poria cocos (Schw.) Wolf triterpenoid extract from Poria cocos (Schw.) Wolf skin, and improve the added value of Poria cocos (Schw.) Wolf skin.

[0005] The technical scheme of the present application is implemented as follows: the present application provides a method for comprehensively utilizing Poria cocos (Schw.) Wolf skin, which comprises the following steps: (1) taking Poria cocos (Schw.) Wolf skin decoction pieces, adding water to decoct and extract, filtering to obtain water extract and residues; (2) Take the water extract in step (1), concentrate, dry, add appropriate excipients to granulate, and make into Poria cocos skin formula granules; (3) Take the residues in step (1), drain the residual water, add ethanol solution, heat reflux extraction, filter, take the filtrate, concentrate and stand, wait for the precipitate to separate out, filter, take the filter residue, and dry to obtain Poria cocos triterpene crude extract; (4) Take the Poria cocos triterpene crude extract in step (3), add ethanol solution, heat or ultrasonic dissolution, stand and crystallize, wait for the precipitate to separate out, filter, take the filter residue, and dry to obtain Poria cocos triterpene refined extract.

[0006] In some embodiments, the specific method of water decoction extraction in step (1) is as follows: first add 10-8 times the volume of water, soak for 30-60 minutes, heat to boiling of the system (temperature 95-100°C), and decoct at 95-100°C for 30-90 minutes; secondly, add 8-6 times the volume of water, heat to boiling of the system (temperature 95-100°C), and decoct at 95-100°C for 30-60 minutes.

[0007] In some embodiments, the specific method of water decoction extraction in step (1) is as follows: first add 10 times the volume of water, soak for 30 minutes, heat to boiling of the system (temperature 100°C), and decoct at 100°C for 60 minutes; secondly, add 8 times the volume of water, heat to boiling of the system (temperature 100°C), and decoct at 100°C for 40 minutes.

[0008] In some embodiments, the concentration in step (2) is concentrated to a relative density of 1.05-1.25 at 60-70°C, the drying method is spray drying, the excipient is malt dextrin, and the granulation method is dry granulation.

[0009] In some embodiments, the ethanol solution in step (3) is 95% ethanol, and the amount added is 6-8 times the volume of the medicinal material; the temperature of heat reflux extraction is 78-82°C, and the extraction time is 2 hours; and the concentration is concentrated to one-half to one-third of the original filtrate volume at 60-75°C.

[0010] In some embodiments, the amount of 95% ethanol added in step (3) is 6 times the volume of the medicinal material, the temperature of heat reflux extraction is 80°C, and the concentration is concentrated to one-half to one-third of the original filtrate volume at 65°C; and the filtration after heat reflux extraction is hot filtration.

[0011] In some embodiments, the concentration of the ethanol solution in step (4) is 60-80%, and the amount added is 5-10 times the amount of the Poria cocos triterpene crude extract; and the temperature of heat dissolution is 80°C.

[0012] In some embodiments, the concentration of the ethanol solution in step (4) is 70%, the amount of ethanol solution added is 8 times the mass of the crude extract of poria cocos triterpenes, the dissolution method is heating at 80 DEG C or ultrasonic dissolution, and the standing time for standing crystallization is 24-48 hours.

[0013] In some embodiments, the residue after draining the residual moisture in step (3) is wet residue, which does not need additional drying treatment and can be directly used for subsequent ethanol solution extraction.

[0014] In some embodiments, the refined extract of poria cocos triterpenes obtained in step (4) can be further separated and purified to obtain monomer substances of poria cocos triterpenes.

[0015] The present application has the following beneficial effects compared with the prior art: The present application realizes efficient comprehensive utilization of poria cocos skin resources, can simultaneously produce two high-value-added products, poria cocos skin formula granules and poria cocos triterpene extract, from the same batch of poria cocos skin decoction pieces, breaks through the limitation of the prior art that poria cocos skin is only used to produce formula granules or extract triterpenes, and significantly improves the economic value of poria cocos skin. The present application provides a new way for processing the residue after producing poria cocos skin formula granules, which avoids the waste of high content of triterpenes in the residue by preparing poria cocos triterpene extract from the residue, and avoids the risk of the residue flowing into the market again. In the whole process, only water and ethanol are used as extraction solvents, without using any toxic and harmful reagents, which conforms to the production concept of low carbon and environmental protection, and reduces the impact on the environment. The present application uses the residue after water extraction of poria cocos skin to prepare poria cocos triterpene extract, which has higher extraction efficiency and higher triterpene content in the extract compared with directly extracting triterpenes from poria cocos skin, simplifies the extraction process steps, reduces the consumption of raw materials and cost input in the production process, and is more convenient for industrialized scale production by pharmaceutical production enterprises. In addition, the refined extract of poria cocos triterpenes can be further purified to obtain monomer components, which lays a foundation for the deep development and utilization of poria cocos triterpenes. BRIEF DESCRIPTION OF DRAWINGS In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed in the following embodiment or prior art description will be briefly introduced. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creating labor.

[0016] Figure 1 The present application is a comprehensive utilization method of poria cocos skin. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative work fall within the scope of protection of the present application.

[0018] Example 1 Preparation step Step 1: water extraction treatment Take 200 g of Poria cocos peel decoction pieces, add 10 times the volume (2000 mL) of purified water for the first time, soak for 30 minutes, then heat to 100°C to boil the system, keep boiling state for 60 minutes, filter with a 200 mesh filter bag, collect the first water extract; add 8 times the volume (1600 mL) of purified water to the filtered residue, heat to 100°C again to boil, keep boiling state for 40 minutes, filter with a 200 mesh filter bag, collect the second water extract; combine the two water extracts for standby.

[0019] Step 2: Poria cocos peel formula granule preparation Transfer the combined water extract to a rotary evaporator, concentrate to a clear paste with a relative density of 1.15 (60°C hot measurement) under the condition of 65°C and -0.08 MPa; send the clear paste to a spray dryer, set the inlet air temperature to 180°C and the outlet air temperature to 80°C for spray drying, obtain dry paste powder; add malt dextrin (malt dextrin mass is 30% of dry paste powder mass) to the dry paste powder, mix uniformly, then use a dry granulation machine (pressure 15 MPa, rotation speed 20 r / min) to granulate, obtain Poria cocos peel formula granules, standby. Step 3: alcohol extraction treatment of residue (two groups for comparison of alcohol extraction times) The filtered residue in step 1 (wet residue mass is about 575 g) is divided into two groups: Group 1 (the present application): add 8 times the volume (1600 mL, based on the mass of decoction pieces) of 95% ethanol to the wet residue, transfer to a round-bottom flask, heat to reflux and slightly boil for 2 hours under the condition of 80°C water bath, filter while hot with a 200 mesh filter bag, collect the alcohol extract filtrate; transfer the filtrate to a rotary evaporator, concentrate to 1 / 3 of the original filtrate volume under the condition of 65°C and -0.09 MPa, stop concentrating; transfer the concentrated liquid to a conical flask, stand at room temperature for 24 hours, filter with filter paper after white precipitate is precipitated, collect the filter residue; dry the filter residue in a 60°C vacuum drying oven to constant weight, obtain Poria cocos triterpene crude extract.

[0020] Group 2 (control group): the first alcohol extraction operation is the same as group 1, and the drug residue after the first alcohol extraction is collected; 6 times the volume (1200 mL based on the mass of the decoction piece) of 95% ethanol is added to the drug residue, and the mixture is heated to reflux and extracted at 80°C for 2 hours; while hot, filter the mixture, and collect the second alcohol extraction filtrate; the subsequent concentration, standing, filtration, and drying operations are the same as group 1, and the second crude triterpene extract of Poria cocos is obtained.

[0021] Performance verification (1) Determination of the extract yield of the formula granules: weigh the mass of the final Poria cocos skin formula granules, and calculate the extract yield according to the formula "extract yield = (formula granule mass / initial mass of Poria cocos skin decoction piece) x 100%".

[0022] (2) Determination of the yield of the crude triterpene extract of Poria cocos: weigh the dry weight of the crude triterpene extract of Poria cocos from each group, and calculate the yield according to the formula "yield = (dry weight of the crude extract / initial mass of the Poria cocos skin decoction piece) x 100%".

[0023] (3) Determination of the triterpene content of Poria cocos: refer to the method "Determination of total triterpenes in health food" in "Technical Guidelines for the Physical and Chemical and Hygienic Index Testing and Evaluation of Health Food (2020 Edition)", use vanillin-glacial acetic acid colorimetry to determine the absorbance at 548 nm, and calculate the total triterpene content.

[0024] (4) Energy consumption and cost estimation: record the ethanol consumption and heating time during the alcohol extraction process, and estimate the ethanol cost and energy consumption cost per unit of raw material according to the unit price of ethanol (8 yuan / L) and electricity cost (1 yuan / degree) in industrial production.

[0025] Results

[0026] This example focuses on the feasibility verification of the "two water extraction and one alcohol extraction" core process, and the results show that: first, the two water extraction parameters (10 times water for the first extraction, 30 min soaking, and 100°C decoction for 60 min; 8 times water for the second extraction, and 100°C decoction for 40 min) can effectively dissolve the water-soluble components in Poria cocos skin, and the extract yield of the obtained formula granules is 4.25%, which meets the national standard of 2%~5.5% extract yield requirement in "Poria cocos skin formula granule quality standard", and meets the production quality requirements of formula granules; secondly, the comparison of the number of alcohol extraction of the drug residue shows that one alcohol extraction can obtain a crude extract with a yield of 3.80% and a total triterpene content of 62.46%, while the yield of two alcohol extraction is only 19.7% of one alcohol extraction, and the ethanol consumption and energy consumption cost increase by 75% and 77% respectively, and the triterpene content does not increase significantly.

[0027] Example 2 Preparation steps Step 1: water extraction and formula granule preparation Take Poria cocos skin decoction pieces 2000 g (2 kg), the first 10 times the volume (20000 ml) of purified water, soaked for 30 minutes, heated to 100 ℃ boiling, decoction 60 minutes, filtration; to the dregs added 8 times the volume (16000 ml) of purified water, 100 ℃ boiling decoction 40 minutes, filtration, combined two times water extract; water extract in 65 ℃, -0.08 MPa under the condition of relative density 1.15 (60 ℃ hot measurement), spray drying (into wind 180 ℃, out of wind 80 ℃), add dry paste powder mass 30% of malt dextrin, dry granulation (pressure 15 MPa, rotation speed 20 r / min), get Poria cocos skin formula granules, for use.

[0028] Step 2: dregs alcohol extraction (two groups compared with ethanol dosage) The filtered dregs of step 1 were drained of residual water (wet dregs mass about 5760 g), and divided into two groups: Group 1: 6 times the volume (based on the mass of decoction pieces, 12000 ml) of 95% ethanol was added to the wet dregs, which were transferred to a 20 L reaction kettle, and extracted by hot reflux micro boiling at 80 ℃ for 2 hours. The filtrate was concentrated to 1 / 3 of the original volume at 65 ℃ under -0.09 MPa, and then left to stand at room temperature for 24 hours. The filter residue was collected and dried at 60 ℃ under vacuum to constant weight to obtain the crude triterpene extract of Poria cocos.

[0029] Group 2: 8 times the volume (based on the mass of decoction pieces, 16000 ml) of 95% ethanol was added to the wet dregs, and the rest of the alcohol extraction, concentration, standing, filtration, and drying operations were the same as those of group 1 to obtain the crude triterpene extract of Poria cocos.

[0030] Performance verification (1) Formula granule extraction rate determination: calculated according to "extraction rate = (formula granule mass / Poria cocos skin decoction piece initial mass) × 100%".

[0031] (2) Yield and content determination of crude triterpene extract of Poria cocos: same as the yield calculation and total triterpene content determination method of Example 1.

[0032] (3) Ethanol cost estimation: calculated the ethanol cost per unit of raw material according to the unit price of ethanol of 8 yuan / L.

[0033] Results

[0034] This example aimed to optimize the ethanol dosage in the alcohol extraction of dregs. The results showed that the yield of crude triterpene extract of Poria cocos (3.48% vs 3.56%) and the total triterpene content (63.94% vs 64.12%) had very small differences (0.08 percentage points difference in yield and 0.12 percentage points difference in purity) between the 6 times volume 95% ethanol group and the 8 times volume group, but the ethanol cost of the 6 times volume group was reduced by 32 yuan.

[0035] Example 3 Preparation step Step 1: Poria cocos triterpenoids crude extract preparation Take 10g of Poria cocos triterpenoids crude extract prepared in Example 2 Group 1 (total triterpenoids content 63.94% by detection), ready for use.

[0036] Step 2: Poria cocos triterpenoids refined extract preparation (two groups compared with refined ethanol concentration) Group 1: Add 8 times the volume (80ml) of 70% ethanol solution to 10g of crude extract, transfer to beaker, 80℃ water bath heating and stirring until completely dissolved; transfer the dissolved solution to a conical flask, stand at room temperature for 48 hours, after the light yellow crystals precipitate, filter paper filtration, collect the filter residue; 60℃ vacuum drying to constant weight, get Poria cocos triterpenoids refined extract.

[0037] Group 2: Add 8 times the volume (80ml) of 50% ethanol solution to 10g of crude extract, the rest of the solution, standing, filtration, drying operation same as group 1, get Poria cocos triterpenoids refined extract.

[0038] Performance verification (1) Refined extract yield determination: according to "refined extract yield = (refined extract dry weight / crude extract initial mass) x 100%" calculation.

[0039] (2) Total triterpenoids content determination of refined extract: same as the total triterpenoids content determination method of Example 1.

[0040] Results

[0041] This example aims to verify the refining process of Poria cocos triterpenoids crude extract, the core comparison of 70% and 50% ethanol refining effect: the total triterpenoids content of refined extract obtained by 70% ethanol group reaches 83.96%, while the purity of 50% ethanol group is only 71.50%, the difference is due to 70% ethanol can better, more dissolved residual impurities (such as a small amount of fat, pigment) in crude extract, at the same time ensure the high efficiency of liposoluble triterpenoids components precipitation.

[0042] Example 4 Preparation step Take 200g of Poria cocos skin decoction pieces, divide into two groups, and process with different process sequence: Group 1 (the present invention, water extraction first and then alcohol extraction): 10 times volume (2000 mL) of purified water was added first, and after soaking for 30 minutes, it was boiled and decocted at 100°C for 60 minutes, and then filtered; 8 times volume (1600 mL) of purified water was added to the residue, and it was boiled and decocted at 100°C for 40 minutes, and then filtered, and the water extracts were combined; the water extracts were granulated according to step 2 of Example 1 to obtain Poria cocos skin formula granules; the residue was dried, 6 times volume (1200 mL) of 95% ethanol was added, and it was hot refluxed at 80°C for 2 hours, and then concentrated, left to stand, filtered, and dried according to Example 1 to obtain Poria cocos triterpenoid crude extract.

[0043] Group 2 (control group, direct alcohol extraction): 6 times volume (1200 mL) of 95% ethanol was added to Poria cocos skin decoction pieces, soaked for 30 minutes, and then hot refluxed at 80°C for 2 hours, and then filtered; the alcohol extract was concentrated, left to stand, filtered, and dried according to Example 1 to obtain Poria cocos triterpenoid crude extract, which was granulated according to step 2 of Example 1 to obtain Poria cocos skin formula granules.

[0044] Performance verification The yield of Poria cocos triterpenoid crude extract and the determination method of total triterpenoid content were the same as in Example 1.

[0045] Results

[0046] This example reveals the key influence of the content of Poria cocos triterpenoid crude extract by comparing the "water extraction first and then alcohol extraction" and "direct alcohol extraction" processes: the yield of crude extract was 3.8%, the total triterpenoid content was 62.46%, and the net content of Poria cocos total triterpenoid was 4.75g in the water extraction first and then alcohol extraction group; the yield of crude extract was 4.05%, but the total triterpenoid content was only 51.20%, and the net content of Poria cocos total triterpenoid was only 4.14g in the direct alcohol extraction group, which was lower than the water extraction first and then alcohol extraction group, and the content was lower, which was not conducive to subsequent purification. It shows that water extraction first and then alcohol extraction has obvious advantages.

[0047] Example 5 Preparation steps Step 1: water extraction treatment Take 200g of Poria cocos skin decoction pieces, add 10 times volume (2000 mL) of purified water first, soak for 30 minutes, and then boil and decoct at 100°C for 60 minutes, and then filter; add 8 times volume (1600 mL) of purified water to the residue, and boil and decoct at 100°C for 40 minutes, and then filter, and collect the residue for use.

[0048] Step 2: residue treatment and alcohol extraction (comparison of dry and wet states in two groups) Group 1: The dregs were drained of residual moisture (wet dregs mass about 288 g), directly added to 8 times volume (1600 mL) of 95% ethanol, hot refluxed at 80°C for 2 hours, and filtered while hot; the filtrate was concentrated to 1 / 3 of the original volume at 65°C, left to stand at room temperature for 24 hours, and the filter residue was collected and dried to constant weight at 60°C under vacuum to obtain the crude extract of Poria cocos triterpenes; the total time from dregs draining to completion of crude extract drying was recorded, and the energy consumption was estimated at a heating power of 1 kW.

[0049] Group 2: The dregs were dried to constant weight in a 60°C air-drying oven (dry dregs mass about 80 g), and 8 times volume (1600 mL, based on the mass of the decoction pieces) of 95% ethanol was added; the rest of the alcohol extraction, concentration, standing, filtration, and drying operations were the same as in Group 1 to obtain the crude extract of Poria cocos triterpenes; the total time was recorded and the energy consumption was estimated.

[0050] Performance verification (1) Crude extract yield and content determination of Poria cocos triterpenes: same as in Example 1.

[0051] (2) Process index recording: The total time from the start of dregs processing to the end of crude extract drying was recorded, and the energy consumption was estimated according to “Energy consumption = power x time” (power taken as 1 kW).

[0052] Results

[0053] This example focuses on the effect of the dry and wet states of the dregs on the extraction process, and the results show that there is no significant difference in the crude extract yield (3.78% vs 3.79%) and total triterpene content (62.40% vs 62.45%) between wet dregs extraction and dry dregs extraction, but the total time for wet dregs extraction is shortened by 33% (4h vs 6h), and the energy consumption is reduced by 50% (4kWh vs 6kWh).

[0054] Comparative Example 1 Preparation steps Step 1: One-time water extraction treatment Take 200 g of Poria cocos skin decoction pieces, add 10 times volume (2000 mL) of purified water, soak for 30 minutes, then heat to 100°C and boil for 60 minutes, filter with a 200-mesh filter bag to collect the water extract (only one-time water extraction); the dregs were drained of residual moisture and reserved.

[0055] Step 2: Formula granules and triterpene extraction The aqueous extract was concentrated to a relative density of 1.15 at 65℃ and -0.08MPa (measured at 60℃), spray-dried (inlet air 180℃, outlet air 80℃), and 30% by weight of maltodextrin was added. The extract was then granulated by dry granulation (pressure 15MPa, rotation speed 20r / min) to obtain Poria cocos peel granules. Eight times the volume (1600mL) of 95% ethanol was added to the residue, and the mixture was refluxed at 80℃ for 2 hours. Subsequent concentration, settling, filtration, and drying were performed as in Example 1 to obtain a crude extract of Poria cocos triterpenes.

[0056] Performance verification The same method was used to determine the granule yield, crude extract yield of Poria cocos triterpenes, and total triterpenoid content as in Example 1.

[0057] result

[0058] This comparative example, by comparing "one-time water extraction" with the "two-time water extraction" of this invention, reveals the key role of the number of water extractions: the granule yield of the formula in the one-time water extraction group was 3.50% (lower than 4.25% in the two-time water extraction group), indicating that the water-soluble components were not fully dissolved; the total content of the crude triterpenoid extract obtained by alcohol extraction of the residue was 52.85% (9.61 percentage points lower than that of the two-time water extraction group), because the one-time water extraction group did not completely remove water-soluble impurities (such as polysaccharides and small molecule organic acids). These impurities co-dissolve with triterpenoid components in ethanol, resulting in a decrease in the purity of the extract.

[0059] Comparative Example 2 Preparation steps Step 1: Direct alcohol extraction Take 200g of Poria cocos peel slices, do not extract with water, directly add 8 times the volume (1600mL) of 80% ethanol, soak for 30 minutes, then extract by hot reflux and gentle boiling in an 80℃ water bath for 2 hours, filter with filter paper while hot, and collect the ethanol extract.

[0060] Step 2: Preparation of crude triterpenoid extract The alcohol extract was concentrated to 1 / 3 of its original volume at 65℃ and -0.09MPa, and allowed to stand at room temperature for 24 hours. After precipitation, the extract was filtered through filter paper and the residue was collected. The residue was then dried under vacuum at 60℃ to constant weight to obtain the crude extract of Poria cocos triterpenes.

[0061] Performance verification The same method was used for determining the crude extraction yield and total triterpenoid content of Poria cocos as in Example 1.

[0062] result

[0063] The comparative example highlights the purity advantage of the alcohol extraction of the drug residue by comparing the "direct 80% ethanol extraction of Poria cocos skin" with the "water extraction and alcohol extraction of the drug residue" of the present application: the yield of triterpenoid crude extract of the direct alcohol extraction group is 5.64% (higher than 3.80% of the alcohol extraction of the drug residue), but the total triterpenoid content is only 45.77% (16.69 percentage points lower than the alcohol extraction of the drug residue), the core reason is that the water-soluble impurities (such as polysaccharides, pigments) in Poria cocos skin are dissolved together with triterpenoid components during direct alcohol extraction, resulting in a significant reduction in the purity of the extract.

[0064] Comparative Example 3 Preparation steps Step 1: Direct 95% ethanol extraction Take Poria cocos skin decoction pieces 200g, do not water extract, directly add 8 times the volume (1600mL) of 95% ethanol, soak for 30 minutes, then extract under reflux at 80℃ water bath for 2 hours, filter with filter paper while hot, collect the alcohol extract.

[0065] Step 2: Preparation of triterpenoid crude extract Concentrate the alcohol extract to 1 / 3 of the original volume at 65℃ and -0.09MPa, stand at room temperature for 24 hours, after the precipitate is precipitated, filter with filter paper, collect the filter residue; dry to constant weight at 60℃ under vacuum to obtain Poria cocos triterpenoid crude extract.

[0066] Performance verification The yield and total triterpenoid content of the Poria cocos triterpenoid crude extract of Example 1 were determined by the same method.

[0067] Results

[0068] This comparative example further verifies the difference between "high concentration ethanol direct extraction" and "drug residue alcohol extraction" of the present application: even if 95% high concentration ethanol is used for direct extraction, the total content of Poria cocos triterpenoid crude extract is still only 55.86% (6.6 percentage points lower than the alcohol extraction of the drug residue), and the yield is 5.06% (higher than the alcohol extraction of the drug residue but the purity disadvantage is significant).

[0069] Comparative Example 4 Preparation steps Step 1: Water extraction and dry residue preparation Take Poria cocos skin decoction pieces 200g, add 10 times the volume (2000mL) of purified water for the first time, soak for 30 minutes, then boil and decoct at 100℃ for 60 minutes, filter; add 8 times the volume (1600mL) of purified water to the drug residue, boil and decoct at 100℃ for 40 minutes, filter; dry the drug residue in a 60℃ air-drying oven to constant weight (the dry residue weighs about 160g), ready for use.

[0070] Step 2: Alcohol extraction of dry residue To the dry residue, 8 times volume (1600 mL, based on the quality of the decoction pieces) of 95% ethanol was added, and hot reflux extraction was performed at 80°C for 2 hours. The filtrate was concentrated to 1 / 3 of the original volume at 65°C, and then left to stand at room temperature for 24 hours. The filter residue was collected by filtration and dried to a constant weight at 60°C under vacuum to obtain the crude extract of Pachymaran. The total time and energy consumption were recorded.

[0071] Performance verification The crude extract yield of Pachymaran, content determination, and process index (time consumption, energy consumption) recording method were the same as those of Example 5.

[0072] Results

[0073] The comparative example further highlights the process advantages of wet residue extraction by comparing "dry residue extraction" with the "wet residue direct extraction" of the present application: there is no significant difference in the crude extract yield of Pachymaran and the content between the two groups, but the dry residue extraction requires an additional 2 hours of drying time, and the energy consumption increases by 50%.

[0074] Comparative Example 5 Preparation steps Step 1: Existing water extraction parameter processing Take 200 g of Pachyma skin decoction pieces, add 12 times volume (2400 mL) of purified water, soak for 60 minutes, then boil at 95°C for 90 minutes, filter with a 200 mesh filter bag, and collect the water extract. The residue was drained and reserved.

[0075] Step 2: Existing alcohol extraction parameter processing To the residue, 10 times volume (2000 mL, based on the quality of the decoction pieces) of 70% ethanol was added, and hot reflux extraction was performed at 70°C for 3 hours. The filtrate was collected by hot filter paper filtration.

[0076] Step 3: Product preparation The water extract was concentrated to a relative density of 1.20 (60°C hot measurement) at 65°C and -0.08 MPa, and then spray dried. The product was granulated with malt dextrin to obtain Pachyma skin formula granules. The alcohol extract was concentrated to 1 / 3 of the original volume at 65°C and -0.09 MPa, and then left to stand at room temperature for 24 hours. The filter residue was collected by filtration and dried at 60°C under vacuum to obtain the crude extract of Pachymaran.

[0077] Performance verification The extract yield of formula granules, the crude extract yield of Pachymaran, and the total triterpenoid content determination method were the same as those of Example 1.

[0078] Results

[0079] This comparative example uses a combination of "existing conventional water extraction parameters + existing alcohol extraction parameters" and compares it with the parameters of this invention: the granule yield of the formula obtained by the existing parameter combination is 3.9% and the total content of crude triterpenoid extract is 48.30%, both of which are significantly inferior to those of this invention (yield 4.25% and triterpenoid content 62.46%).

[0080] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for comprehensive utilization of Poria cocos periderm, characterized in that, It comprises the following steps: (1) Take the Poria cocos skin decoction pieces, add water to extract, filter, and obtain the water extract and residue; (2) Take the water extract in step (1), concentrate, dry, add appropriate amount of excipients to granulate, and prepare Poria cocos skin formula granules; (3) Take the residue in step (1), drain the residual water, add ethanol solution, heat reflux to extract, filter, take the filtrate, concentrate, and stand still until the precipitate is separated out, then filter, take the filter residue, and dry to obtain the Poria cocos triterpene crude extract; (4) Take the Poria cocos triterpene crude extract in step (3), add ethanol solution, heat or ultrasonic to dissolve, stand still to crystallize, wait until the precipitate is separated out, then filter, take the filter residue, and dry to obtain the Poria cocos triterpene refined extract.

2. The method of claim 1, wherein, In step (1), the specific method of water decoction extraction is as follows: add 10-8 times the volume of water for the first time, soak for 30-60 minutes, boil, and decoct at 95-100℃ for 30-90 minutes; add 8-6 times the volume of water for the second time, boil, and decoct at 95-100℃ for 30-60 minutes.

3. The method of claim 2, wherein, In step (1), the specific method of water decoction extraction is as follows: add 10 times the volume of water for the first time, soak for 30 minutes, boil, and decoct at 100℃ for 60 minutes; add 8 times the volume of water for the second time, boil, and decoct at 100℃ for 40 minutes.

4. The method of claim 1, wherein, In step (2), the concentration is at 60-70℃ to concentrate to the relative density of 1.05-1.25, the drying is spray drying, the excipient is malt dextrin, and the granulation is dry granulation.

5. The method of claim 1, wherein, In step (3), the ethanol solution is 95% ethanol, and its addition amount is 6-8 times the volume of the decoction pieces; the temperature of heat reflux extraction is 78-82℃, and the extraction time is 2 hours; and the concentration is at 60-75℃ to concentrate to one-half to one-third of the volume of the original filtrate.

6. The method of claim 5, wherein, In step (3), the addition amount of 95% ethanol is 6 times the volume of the decoction pieces, the temperature of heat reflux extraction is 80℃, and the concentration is at 65℃ to concentrate to one-half to one-third of the volume of the original filtrate.

7. The method of claim 1, wherein, In step (4), the concentration of the ethanol solution is 60-80%, and its addition amount is 5-10 times the mass of the Poria cocos triterpene crude extract; and the temperature of heating dissolution is 80℃.

8. The method of claim 7, wherein, In step (4), the concentration of the ethanol solution is 70%, its addition amount is 8 times the mass of the Poria cocos triterpene crude extract, and the dissolution method is heating or ultrasonic dissolution at 80℃.

9. The method of claim 1, wherein, In step (3), the filtration after heat reflux extraction is hot filtration.

10. The method of claim 7, wherein, In step (4), the standing time of standing crystallization is 24-48 hours.

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