Method for refining and desalting belladonna fluid extract

Abstract

This invention discloses a method for refining and desalting belladonna fluid extract, relating to the field of traditional Chinese medicine pharmaceuticals. Belladonna grass is pulverized through a 24-mesh sieve to form coarse powder. The powder is percolated using ethanol as a solvent to obtain a primary belladonna extract. The ethanol is recovered from the primary extract, and the extract is cooled to room temperature. Chlorophyll is removed by separation using a ceramic membrane. The extract is then filtered, and the filtrate is concentrated using an organic nanofiltration membrane to remove salts. The membrane filtrate is further concentrated under reduced pressure to a thick paste. Seven times the volume of ethanol is added and stirred until homogeneous. The mixture is allowed to stand until complete precipitation. The supernatant is collected, and the ethanol is recovered and concentrated to a thick paste. Based on the content determined in the thick paste, an appropriate amount of 85% ethanol is added, and the mixture is diluted with water to prepare a finished belladonna fluid extract product conforming to pharmacopoeia standards. This method is stable and reliable, avoids high-temperature degradation of the active ingredients, effectively removes impurities from the belladonna fluid extract, and prevents salt precipitation in the finished product. This ensures its efficacy and medication safety, and has broad market application prospects.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine manufacturing, specifically to a method for refining and desalting belladonna fluid extract. Background Technology

[0002] Belladonna extract is a fluid extract made from the belladonna plant. It has a slightly foul odor and is a postganglionic anticholinergic drug that blocks M receptors. It has the effects of relieving smooth muscle spasms and inhibiting glandular secretion. It is suitable for gastric and duodenal ulcers, gastrointestinal, renal, and biliary colic.

[0003] Current observations of belladonna extract under refrigeration show that a small amount of salt precipitates at the bottom of the extract. As a major component of joint pain relief ointments, this salt precipitation affects the ointment's production and can cause skin irritation. This invention utilizes a refining and desalting process to significantly reduce the total solids of belladonna extract and remove a large amount of salt from the belladonna plant, thus preventing salt precipitation. This process also avoids the loss of key active ingredients caused by prolonged high-temperature concentration and improves the yield of hyoscyamine sulfate. Summary of the Invention

[0004] The purpose of this invention is to solve the problem of salt leaching from belladonna extract, reduce total solids, and provide a method for refining and desalting belladonna extract.

[0005] The technical solution of the present invention is as follows:

[0006] A method for refining and desalting belladonna fluid extract involves percolating coarse belladonna powder with a percolating solvent to obtain a percolate, recovering ethanol, removing chlorophyll using a ceramic membrane, concentrating the filtrate through an organic nanofiltration membrane to obtain a desalted concentrate, further concentrating under reduced pressure to a thick paste, adding ethanol and stirring evenly, allowing it to stand, aspirating the supernatant, recovering ethanol to a thick paste, and adding 85% vol% ethanol and water to prepare belladonna fluid extract.

[0007] As a preferred embodiment of the present invention, the organic nanofiltration membrane is further subjected to the following treatment:

[0008] The organic nanofiltration membrane is modified by immersing it in a treatment solution, then removed, dried, and then placed in a dendritic polyether solution containing inorganic nanoparticles. After removal, it is immersed in an organic phase and finally subjected to a crosslinking reaction at 70-150℃ to obtain the final product.

[0009] As a preferred embodiment of the present invention, the treatment solution is prepared by dissolving sodium alginate and polyvinyl alcohol in deionized water.

[0010] As a preferred embodiment of the present invention, the inorganic nanoparticles are silicon dioxide, accounting for 1-5 wt% of the dendritic polyether solution;

[0011] The dendritic polyether solution is prepared by mixing potassium carbonate, 3,5-dihydroxybenzyl alcohol, crown ether and acetone, adding benzyl chloride and reacting for 40-48 hours. After the reaction is completed, the acetone is evaporated, dissolved in dichloromethane, and the organic phase is collected.

[0012] As a preferred embodiment of the present invention, the belladonna powder is belladonna grass that has been crushed and passed through a 20-30 mesh sieve.

[0013] As a preferred embodiment of the present invention, the percolation solvent is ethanol with a volume fraction of 70-90%.

[0014] As a preferred embodiment of the present invention, the pore size of the ceramic membrane is 200-600 nm.

[0015] As a preferred embodiment of the present invention, the volume ratio of the desalted concentrate to the filtrate is 1:2-3.

[0016] As a preferred embodiment of the present invention, the organic nanofiltration membrane has a molecular weight cutoff of 150-500 Daltons.

[0017] As a preferred embodiment of the present invention, in the step of adding ethanol and stirring evenly, the volume ratio of ethanol to thick paste is 4-10:1; the volume fraction of ethanol is 85-95%.

[0018] The beneficial effects of this invention are:

[0019] (1) A method for refining and desalting belladonna fluid extract according to the present invention uses organic nanofiltration concentration process to desalt belladonna filtrate, which can significantly remove impurities in the medicine solution, thereby improving the clarity of the medicine solution and avoiding the possibility of salt precipitation, improving the safety of belladonna fluid extract, and avoiding the risk of salt precipitation during the preparation of the plaster.

[0020] (2) The present invention provides a method for refining and desalting belladonna fluid extract. By using a suitable nanofiltration membrane with a molecular weight cutoff of 150-500 Daltons, especially 200 Daltons, the loss of active ingredients can be reduced, and the degradation of active ingredients caused by prolonged heating can be avoided. This method can significantly improve the yield of hyoscyamine sulfate.

[0021] (3) A method for refining and desalting belladonna extract according to the present invention improves the water flux and retention rate by forming a loose and porous hydrophilic layer on the base membrane and then forming a dense active layer of inorganic nanoparticles through hybrid interpenetration. Detailed Implementation

[0022] The technical solution of the present invention will be further described below with reference to specific embodiments.

[0023] Example 1

[0024] A method for refining and desalting belladonna fluid extract involves crushing belladonna grass through a 24-mesh sieve to obtain coarse powder, percolating with 85% (v / v) ethanol as a solvent to obtain a filtrate, recovering the ethanol, removing chlorophyll using a ceramic membrane, concentrating the filtrate through an organic nanofiltration membrane (sodium polyacrylonitrile membrane) to remove salts, further concentrating under reduced pressure to a thick paste, adding 95% (v / v) ethanol and stirring evenly, allowing it to stand overnight, collecting the supernatant, recovering the ethanol to a thick paste, and adding appropriate amounts of 85% (v / v) ethanol and water to prepare a qualified belladonna fluid extract.

[0025] The organic nanofiltration concentration ratio is 1:2, where the volume ratio of concentrate to filtrate is 1:2.

[0026] The ceramic membrane used to remove chlorophyll employs a ceramic membrane with a pore size of 200 nanometers.

[0027] The organic nanofiltration concentration uses a molecular weight cutoff of 200 Daltons.

[0028] Example 2

[0029] A method for refining and desalting belladonna fluid extract involves crushing belladonna grass through a 24-mesh sieve to obtain coarse powder, percolating with 85% (v / v) ethanol as a solvent to obtain a filtrate, recovering the ethanol, removing chlorophyll using a ceramic membrane, concentrating the filtrate through an organic nanofiltration membrane (sodium polyacrylonitrile membrane) to remove salts, further concentrating under reduced pressure to a thick paste, adding 95% (v / v) ethanol and stirring evenly, allowing it to stand overnight, collecting the supernatant, recovering the ethanol to a thick paste, and adding appropriate amounts of 85% ethanol and water to prepare a qualified belladonna fluid extract.

[0030] The organic nanofiltration concentration ratio is 1:2, where the volume ratio of concentrate to filtrate is 1:2.

[0031] The ceramic membrane used to remove chlorophyll employs a ceramic membrane with a pore size of 200 nanometers.

[0032] The organic nanofiltration concentration uses a molecular weight cutoff of 300 Daltons.

[0033] Example 3

[0034] A method for refining and desalting belladonna extract: Belladonna grass is crushed through a 24-mesh sieve to obtain coarse powder. It is then percolated with 85% (v / v) ethanol as a solvent to obtain a percolate. The ethanol is recovered, and chlorophyll is removed using a ceramic membrane. The filtrate is then concentrated through an organic nanofiltration membrane (sodium polyacrylonitrile membrane) to remove salts. Further concentration under reduced pressure is carried out to a thick paste. 95% (v / v) ethanol is added and stirred until homogeneous. The mixture is allowed to stand overnight, and the supernatant is collected. The ethanol is recovered to a thick paste. Appropriate amounts of 85% ethanol and water are added to prepare a qualified belladonna extract.

[0035] The organic nanofiltration concentration ratio is 1:2, where the volume ratio of concentrate to filtrate is 1:2.

[0036] The ceramic membrane used to remove chlorophyll employs a ceramic membrane with a pore size of 200 nanometers.

[0037] The organic nanofiltration concentration uses a molecular weight cutoff of 500 Daltons.

[0038] Example 4

[0039] A method for refining and desalting belladonna fluid extract involves crushing belladonna grass through a 24-mesh sieve to obtain coarse powder, percolating with 85% (v / v) ethanol as a solvent to obtain a filtrate, recovering the ethanol, removing chlorophyll using a ceramic membrane, concentrating the filtrate through an organic nanofiltration membrane (sodium polyacrylonitrile membrane) to remove salts, further concentrating under reduced pressure to a thick paste, adding 95% (v / v) ethanol and stirring evenly, allowing it to stand overnight, collecting the supernatant, recovering the ethanol to a thick paste, and adding appropriate amounts of 85% ethanol and water to prepare a qualified belladonna fluid extract.

[0040] The organic nanofiltration concentration ratio is 1:3, where the volume ratio of concentrate to filtrate is 1:3.

[0041] The ceramic membrane used to remove chlorophyll employs a ceramic membrane with a pore size of 200 nanometers.

[0042] The organic nanofiltration concentration uses a molecular weight cutoff of 200 Daltons.

[0043] Example 5

[0044] A method for refining and desalting belladonna fluid extract involves crushing belladonna grass through a 24-mesh sieve to obtain coarse powder, percolating with 85% (v / v) ethanol as a solvent to obtain a filtrate, recovering the ethanol, removing chlorophyll using a ceramic membrane, concentrating the filtrate through an organic nanofiltration membrane (sodium polyacrylonitrile membrane) to remove salts, further concentrating under reduced pressure to a thick paste, adding 95% (v / v) ethanol and stirring evenly, allowing it to stand overnight, collecting the supernatant, recovering the ethanol to a thick paste, and adding appropriate amounts of 85% ethanol and water to prepare a qualified belladonna fluid extract.

[0045] The organic nanofiltration concentration ratio is 1:4, where the volume ratio of concentrate to filtrate is 1:4.

[0046] The ceramic membrane used to remove chlorophyll employs a ceramic membrane with a pore size of 200 nanometers.

[0047] The organic nanofiltration concentration uses a molecular weight cutoff of 200 Daltons.

[0048] Example 6

[0049] This embodiment is a variation based on Example 1. Specifically, the organic nanofiltration membrane (sodium polyacrylonitrile filter membrane) is modified by immersing it in a treatment solution, then removed, dried, and then placed in a dendritic polyether solution containing inorganic nanoparticles. After removal, it is immersed in an organic phase and finally subjected to a crosslinking reaction at 120°C to obtain the final product.

[0050] The treatment solution is prepared by dissolving sodium alginate and polyvinyl alcohol in deionized water at a mass ratio of 3:1.

[0051] The inorganic nanoparticles are silicon dioxide, accounting for 2 wt% of the dendritic polyether solution;

[0052] The dendritic polyether solution was prepared by mixing 0.37 mol potassium carbonate, 0.15 mol 3,5-dihydroxybenzyl alcohol, 0.03 mol crown ether and acetone, adding 0.35 mol benzyl chloride and reacting for 48 h. After the reaction was completed, the acetone was evaporated, dissolved in dichloromethane, and the organic phase was collected.

[0053] Example 7

[0054] This embodiment is a variation based on Example 1. Specifically, the organic nanofiltration membrane (sodium polyacrylonitrile filter membrane) is modified by immersing it in a treatment solution, then removed, dried, and then placed in a dendritic polyether solution containing inorganic nanoparticles. After removal, it is immersed in an organic phase and finally subjected to a crosslinking reaction at 120°C to obtain the final product.

[0055] The treatment solution is prepared by dissolving sodium alginate and polyvinyl alcohol in deionized water at a mass ratio of 3:1.

[0056] The inorganic nanoparticles are silicon dioxide, accounting for 5 wt% of the dendritic polyether solution;

[0057] The dendritic polyether solution was prepared by mixing 0.37 mol potassium carbonate, 0.15 mol 3,5-dihydroxybenzyl alcohol, 0.03 mol crown ether and acetone, adding 0.35 mol benzyl chloride and reacting for 48 h. After the reaction was completed, the acetone was evaporated, dissolved in dichloromethane, and the organic phase was collected.

[0058] Comparative Example 1 (without nanofiltration concentration process)

[0059] A method for refining and desalting belladonna extract involves crushing belladonna grass through a 24-mesh sieve to obtain coarse powder, percolating it with 85% (v / v) ethanol as a solvent to obtain a percolate, recovering the ethanol, removing chlorophyll using a ceramic membrane, concentrating the filtrate under reduced pressure to a thick paste, adding 95% (v / v) ethanol and stirring evenly, allowing it to stand overnight, collecting the supernatant, recovering the ethanol to a thick paste, and adding appropriate amounts of 85% ethanol and water to prepare a qualified belladonna extract.

[0060] The ceramic membrane used to remove chlorophyll employs a ceramic membrane with a pore size of 200 nanometers.

[0061] Comparative Example 2 (No treatment solution)

[0062] This comparative example is a variation of Example 6. Specifically, the organic nanofiltration membrane (sodium polyacrylonitrile filter membrane) was placed in a dendritic polyether solution containing inorganic nanoparticles, then removed and immersed in an organic phase, and finally subjected to a crosslinking reaction at 120°C to obtain the final product.

[0063] The inorganic nanoparticles are silicon dioxide, accounting for 2 wt% of the dendritic polyether solution;

[0064] The dendritic polyether solution was prepared by mixing 0.37 mol potassium carbonate, 0.15 mol 3,5-dihydroxybenzyl alcohol, 0.03 mol crown ether and acetone, adding 0.35 mol benzyl chloride and reacting for 48 h. After the reaction was completed, the acetone was evaporated, dissolved in dichloromethane, and the organic phase was collected.

[0065] The above-described embodiments and comparative examples were used to prepare qualified belladonna fluid extract products. The yields of hyoscyamine sulfate and scopolamine were determined by high-performance liquid chromatography (HPLC), and the total solids of the finished product were also measured. The results are shown in Table 1.

[0066] Table 1. Yields and Total Solids of Indicator Components in Examples and Comparative Examples

[0067]

[0068]

[0069] Based on the overall yield and total solids data, the total solids in the non-desalination process (Comparative Example 1) were significantly higher. The main reason is that the molecular weight cutoff of the nanofiltration membrane is a key factor; a cutoff greater than 200 Daltons resulted in higher permeability of hyoscyamine sulfate and scopolamine, leading to greater losses. Examples 6 and 7 were superior to Examples 1-5. Combined with the analysis of Comparative Example 2, it can be seen that the main reason for the improved desalination rate is that Examples 6 and 7 further modified the organic nanofiltration membrane to form a loose, porous hydrophilic layer, increasing the water flux. Then, a dense active layer of inorganic nanoparticles with interpenetrating hybrid structure was formed, increasing the retention rate of active ingredients.

[0070] The belladonna extracts prepared in the above examples and comparative examples were refrigerated (2-8℃) for 15 months to observe the salt precipitation. See Table 2:

[0071] Table 2. Salt precipitation at different refrigeration times in the examples and comparative examples.

[0072]

[0073]

[0074] The results of Comparative Example 1 show that refining and desalting can prevent salt precipitation. By optimizing various process parameters, no salt precipitation was observed in Examples 1-7 over a period of up to 12 months. Example 6, as a method for refining and desalting belladonna extract, can prepare qualified belladonna extract. During a period of up to 15 months of cold storage, the loss of active ingredients is minimal, and salt precipitation is avoided. This is helpful for the production of ointments, reduces the total solids of belladonna extract, and further improves the quality of belladonna extract.

[0075] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the present invention in any way. Other variations and modifications may be made without departing from the technical solutions described in the claims.

Claims

1. A method for refining and desalting belladonna fluid extract, characterized in that, The coarse powder of belladonna was percolated with a percolating solvent to obtain a filtrate. The ethanol was recovered, and chlorophyll was removed using a ceramic membrane. The filtrate was concentrated through an organic nanofiltration membrane to obtain a salt-free concentrate. The concentrate was further concentrated under reduced pressure to a thick paste. Ethanol was added and stirred evenly. The mixture was allowed to stand, and the supernatant was aspirated. The ethanol was recovered to a thick paste. 85 wt% ethanol and water were added to prepare belladonna fluid extract. The organic nanofiltration concentration uses a sodium polyacrylonitrile membrane with a molecular weight cutoff of 200 Daltons; the organic nanofiltration membrane also undergoes the following treatment: The organic nanofiltration membrane was modified by immersing it in a treatment solution, then removed, dried, and then placed in a dendritic polyether solution containing inorganic nanoparticles. After removal, it was immersed in an organic phase and finally subjected to a crosslinking reaction at 70-150℃ to obtain the final product. The treatment solution is prepared by dissolving sodium alginate and polyvinyl alcohol in deionized water. The inorganic nanoparticles are silicon dioxide, comprising 1-5 wt% of the dendritic polyether solution; The dendritic polyether solution is prepared by mixing potassium carbonate, 3,5-dihydroxybenzyl alcohol, crown ether and acetone, adding benzyl chloride and reacting for 40-48 hours. After the reaction is completed, the acetone is evaporated, dissolved in dichloromethane, and the organic phase is collected.

2. The method for refining and desalting belladonna fluid extract according to claim 1, characterized in that, The belladonna powder is made by crushing belladonna grass and passing it through a 20-30 mesh sieve.

3. The method for refining and desalting belladonna fluid extract according to claim 1, characterized in that, The percolation solvent is ethanol with a volume fraction of 70-90%.

4. The method for refining and desalting belladonna fluid extract according to claim 1, characterized in that, The ceramic membrane has a pore size of 200-600 nm.

5. The method for refining and desalting belladonna fluid extract according to claim 1, characterized in that, The volume ratio of the desalted concentrate to the filtrate is 1:2-3.

6. The method for refining and desalting belladonna fluid extract according to claim 1, characterized in that, In the step of adding ethanol and stirring evenly, the volume ratio of ethanol to thick paste is 4-10:1; the volume fraction of ethanol is 85-95%.

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