Ganoderma lucidum and bitter gourd chromium tablet and preparation method thereof

Abstract

The invention provides a preparation method of ganoderma lucidum and bitter gourd chromium tablets, which comprises the following steps: uniformly mixing a bitter gourd extracting solution, a ganoderma lucidum extracting solution and an imidazole acetic acid ionic liquid, adding an alkaline aqueous solution, filtering after ganoderma lucidum polysaccharide is separated out, adjusting the filtrate to be acidic, adding absolute ethyl alcohol to precipitate charantin, and finally efficiently separating the ganoderma lucidum polysaccharide from the charantin. Ganoderma lucidum polysaccharide, charantin, chromium picolinate, starch and other auxiliary materials are prepared into tablets by a conventional method, namely the ganoderma lucidum and bitter gourd chromium tablets.

Description

Technical Field

[0001] The invention relates to a blood sugar lowering tablet, in particular to a ganoderma lucidum bitter melon chromium tablet and a preparation method thereof. Background Art

[0002] Ganoderma lucidum and bitter melon chromium tablets are a common blood sugar lowering tablet, whose main ingredients are extracts of Ganoderma lucidum and bitter melon.

[0003] Ganoderma lucidum contains a variety of active components such as Ganoderma polysaccharides, which have multiple functions such as improving the body's immunity and anti-oxidation. However, the extraction of Ganoderma polysaccharides currently relies on ultrasonic extraction, water extraction, etc. These methods are time-consuming and have low extraction rates.

[0004] Bitter melon is a plant of the genus Momordica in the Cucurbitaceae family. It is bitter and cold in nature. It has the effects of clearing away heat and cooling down, quenching thirst and inducing drinking. In recent years, people have extracted momordica charantia from bitter melon and used it in the clinical treatment of diabetes, but the purity of the extraction is not high, resulting in poor efficacy.

[0005] In the existing technology, Ganoderma lucidum polysaccharide and momordica charantia are generally extracted separately, and the process time is relatively long. Summary of the Invention

[0006] In order to solve the technical problems existing in the background technology, the present invention provides a preparation method of Ganoderma lucidum and bitter melon chromium tablets, comprising the following steps:

[0007] S1. taking the supernatant of the bitter melon juice to obtain a bitter melon extract;

[0008] S2, obtaining a Ganoderma lucidum extract by ultrasonic extraction;

[0009] S3, adding an alkaline aqueous solution to the mixture of the bitter melon extract, the ganoderma lucidum extract and the imidazole acetate ionic liquid to obtain ganoderma lucidum polysaccharide and a filtrate;

[0010] S4, adjusting the filtrate in step S3 to an acidic filtrate, adding anhydrous ethanol to the acidic filtrate to obtain momordica charantia;

[0011] S5. Prepare tablets from ganoderma lucidum polysaccharide, momordica charantia, chromium picolinate, starch, sodium carboxymethyl starch, silicon dioxide and magnesium stearate.

[0012] In the present invention, unlike traditional methods, the high compatibility of ionic liquids is utilized to simultaneously dissolve Ganoderma lucidum polysaccharides and momordicin, and the polarity difference between the two extracts is utilized to perform step-by-step precipitation, shortening the process time by 50%; the Ganoderma lucidum polysaccharide extract and the momordica charantia extract are both aqueous phase systems, and the imidazole acetate ionic liquid has a certain hydrophilicity, so the three can form a homogeneous mixture.

[0013] In step S1, the supernatant of the bitter melon juice is obtained by filtering the bitter melon juice and then centrifuging it. The centrifugal speed is 6000-8000 rpm and the centrifugal time is 20-40 min.

[0014] In step S2, the ultrasonic extraction method has an ultrasonic power of 150-300 W, an ultrasonic frequency of 50-100 kHz, and an ultrasonic time of 2-5 h.

[0015] In step S3, the mass ratio of the bitter melon extract, the ganoderma lucidum extract and the imidazole acetate ionic liquid is 1:1:0.5.

[0016] In step S3, the volume ratio of the mixture of the bitter melon extract, the ganoderma lucidum extract and the imidazole acetate ionic liquid to the alkaline aqueous solution is 1:2-3.

[0017] In step S3, the pH of the alkaline aqueous solution is 8;

[0018] Preferably, the alkaline aqueous solution is prepared from sodium hydroxide and deionized water.

[0019] In the present invention, the addition of alkaline aqueous solution can enhance the hydrophilicity of Ganoderma lucidum polysaccharide, promote the precipitation of Ganoderma lucidum polysaccharide, and inhibit the ionization of momordica charantia, especially the ionization of carboxyl saponins, and reduce the interaction between Ganoderma lucidum polysaccharide and momordica charantia.

[0020] In step S4, the pH of the acidic filtrate is 5;

[0021] Preferably, the filtrate in step S3 is adjusted to an acidic filtrate by acetic acid.

[0022] In step S4, the volume ratio of the acidic filtrate to anhydrous ethanol is 1:2.3-5.

[0023] In the present invention, the water solubility of momordica charantia can be reduced under weak acid conditions, while avoiding the redissolution of residual Ganoderma lucidum polysaccharides. With the addition of ethanol, when the ethanol content in the acidic filtrate exceeds 70%, momordica charantia precipitates due to the change in the polarity of the solution.

[0024] The ganoderma lucidum polysaccharide and momordica charantia need to be subjected to reduced pressure distillation before being made into tablets.

[0025] In the present invention, the reduced pressure distillation can remove volatile substances (water, ionic liquid, ethanol, etc.).

[0026] The present invention also provides a Ganoderma lucidum and bitter melon chromium tablet, which is prepared by the above preparation method.

[0027] The present invention has the beneficial effects of utilizing the polarity difference between Ganoderma lucidum polysaccharide and momordicin, sequentially adding an aqueous solution and anhydrous ethanol to a hydrophilic ionic liquid to precipitate Ganoderma lucidum polysaccharide and momordicin step by step; adjusting the pH value of the system during the step-by-step precipitation to further improve the separation degree of Ganoderma lucidum polysaccharide and momordicin, ultimately obtaining high-purity Ganoderma lucidum polysaccharide and momordicin, and shortening the process time by 50%. DETAILED DESCRIPTION

[0028] To facilitate understanding of the present invention, the present invention will be described more fully below in conjunction with specific embodiments. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to provide a more thorough and comprehensive understanding of the disclosure of the present invention.

[0029] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0030] The technical solution of the present invention is described more clearly and completely below with reference to specific embodiments and comparative examples.

[0031] Example 1

[0032] This embodiment provides a Ganoderma lucidum bitter melon chromium tablet, the preparation method of which is as follows:

[0033] (1) Wash and squeeze out 5 kg of fresh bitter melon, filter, and centrifuge at 2°C (8000 rpm, 20 min). Take the supernatant to obtain the bitter melon extract, and store it at -4°C for later use;

[0034] (2) 5 kg of Ganoderma lucidum was dissolved in 1000 mL of deionized water and ultrasonicated at 200 W and 50 kHz for 2 h. The ultrasonicated mixture was heated to 80°C and extracted for 2 h. The Ganoderma lucidum extract was filtered and stored at 2°C for later use.

[0035] (3) The bitter melon extract, the ganoderma lucidum extract and 1-butyl-3-methylimidazolium acetate ([Bmim][OAc]) were weighed in a mass ratio of 1:1:0.5, placed in a beaker and stirred for 1 hour to obtain a uniform mixture, the mixture was continued to be stirred and a sodium hydroxide aqueous solution (pH = 8, the volume ratio of the mixture to the sodium hydroxide aqueous solution was 1:2.5) was slowly added dropwise, and the mixture was allowed to stand at 5°C for 1 hour and then ultrafiltered (ultrafiltration membrane 40 kDa molecular weight cutoff) to obtain a filter residue 1 and a filtrate 1, and the filter residue 1 was subjected to reduced pressure distillation at 30°C and a vacuum degree of 0.1 MPa to remove volatile components to obtain a ganoderma lucidum polysaccharide powder with a purity of 87%;

[0036] (4) adding glacial acetic acid to the filtrate 1 to obtain a filtrate 1 with a pH of 5, and then adding anhydrous ethanol solution to make the ethanol content in the filtrate 1 80%. After stirring at 25°C and 100 rpm for 1 hour, ultrafiltration (ultrafiltration membrane 10 kDa molecular weight cutoff) was performed to obtain a filter residue 2 and a filtrate 2. The filter residue 2 was subjected to reduced pressure distillation at 50°C and a vacuum degree of 0.1 MPa to remove volatile components to obtain momordica charantia with a purity of 75%;

[0037] (5) 25 parts of Ganoderma lucidum polysaccharide, 55 parts of momordica charantia, 0.01 parts of chromium picolinate, 14 parts of starch, 3 parts of sodium carboxymethyl starch, 2 parts of silicon dioxide, and 0.99 parts of magnesium stearate were mixed evenly and sterilized by ultraviolet light to prepare tablets of 0.8 g / tablet.

[0038] Example 2

[0039] This embodiment provides a Ganoderma lucidum bitter melon chromium tablet, the preparation method of which is as follows:

[0040] (1) Wash and squeeze out 3 kg of fresh bitter melon, filter, and centrifuge at 3°C ​​(6000 rpm, 20 min). Take the supernatant to obtain the bitter melon extract, and store it at -4°C for later use.

[0041] (2) 4 kg of Ganoderma lucidum was dissolved in 1000 mL of deionized water and ultrasonicated at 200 W and 50 kHz for 2 h. The ultrasonicated mixture was heated to 80°C and extracted for 2 h. The Ganoderma lucidum extract was filtered and stored at 2°C for later use.

[0042] (3) The bitter melon extract, the ganoderma lucidum extract and 1-butyl-3-methylimidazolium acetate ([Bmim][OAc]) were weighed in a mass ratio of 1:1:0.5, placed in a beaker and stirred for 1 hour to obtain a uniform mixture, the mixture was continued to be stirred and a sodium hydroxide aqueous solution (pH = 8, the volume ratio of the mixture to the sodium hydroxide aqueous solution was 1:3) was slowly added dropwise, and the mixture was allowed to stand at 5°C for 1 hour and then ultrafiltered (ultrafiltration membrane 30 kDa molecular weight cutoff) to obtain a filter residue 1 and a filtrate 1, and the filter residue 1 was subjected to reduced pressure distillation at 30°C and a vacuum degree of 0.1 MPa to remove volatile components to obtain a ganoderma lucidum polysaccharide powder with a purity of 83%;

[0043] (4) adding glacial acetic acid to the filtrate 1 to obtain a filtrate 1 with a pH of 6, and then adding anhydrous ethanol solution to make the ethanol content in the filtrate 1 70%, stirring at 25°C at a speed of 100 rpm for 1 hour, and then ultrafiltration (ultrafiltration membrane 20 kDa molecular weight cutoff) to obtain a filter residue 2 and a filtrate 2, and the filter residue 2 was subjected to reduced pressure distillation at 50°C and a vacuum degree of 0.1 MPa to remove volatile components to obtain momordica charantia with a purity of 76%;

[0044] (5) 25 parts of Ganoderma lucidum polysaccharide, 55 parts of momordica charantia, 0.01 parts of chromium picolinate, 14 parts of starch, 3 parts of sodium carboxymethyl starch, 2 parts of silicon dioxide, and 0.99 parts of magnesium stearate were mixed evenly and sterilized by ultraviolet light to prepare tablets of 0.8 g / tablet.

[0045] Example 3

[0046] This embodiment provides a Ganoderma lucidum bitter melon chromium tablet, the preparation method of which is as follows:

[0047] (1) Wash and squeeze out 5 kg of fresh bitter melon, filter, and centrifuge at 2°C (8000 rpm, 20 min). Take the supernatant to obtain the bitter melon extract, and store it at -4°C for later use;

[0048] (2) 5 kg of Ganoderma lucidum was dissolved in 1000 mL of deionized water and sonicated at 150 W and 50 kHz for 3 h. The sonicated mixture was heated to 80°C and extracted for 2 h. The Ganoderma lucidum extract was filtered and stored at 2°C for later use.

[0049] (3) The bitter melon extract, the ganoderma lucidum extract and 1-butyl-3-methylimidazolium acetate ([Bmim][OAc]) were weighed in a mass ratio of 1:1:0.5, placed in a beaker and stirred for 1 hour to obtain a uniform mixture, and the mixture was continued to be stirred and a sodium hydroxide aqueous solution (pH = 8, the volume ratio of the mixture to the sodium hydroxide aqueous solution was 1:2) was slowly added dropwise. After standing at 5°C for 1 hour, ultrafiltration (ultrafiltration membrane 40 kDa molecular weight cutoff) was performed to obtain a filter residue 1 and a filtrate 1. The filter residue 1 was subjected to reduced pressure distillation at 30°C and a vacuum degree of 0.1 MPa to remove volatile components to obtain a ganoderma lucidum polysaccharide powder with a purity of 85%;

[0050] (4) adding glacial acetic acid to the filtrate 1 to obtain a filtrate 1 with a pH of 5, and then adding anhydrous ethanol solution to make the ethanol content in the filtrate 1 85%. After stirring at 25°C and 100 rpm for 1 hour, ultrafiltration (ultrafiltration membrane 10 kDa molecular weight cutoff) was performed to obtain a filter residue 2 and a filtrate 2. The filter residue 2 was subjected to reduced pressure distillation at 50°C and a vacuum degree of 0.1 MPa to remove volatile components, thereby obtaining momordica charantia with a purity of 72%;

[0051] (5) 25 parts of Ganoderma lucidum polysaccharide, 55 parts of momordica charantia, 0.01 parts of chromium picolinate, 14 parts of starch, 3 parts of sodium carboxymethyl starch, 2 parts of silicon dioxide, and 0.99 parts of magnesium stearate were mixed evenly and sterilized by ultraviolet light to prepare tablets of 0.8 g / tablet.

[0052] Comparative Example 1

[0053] This comparative example provides a Ganoderma lucidum bitter melon chromium tablet, the preparation method of which is the same as that of Example 1, except that the step (3) of "continue stirring the mixture and slowly dropwise add sodium hydroxide aqueous solution (pH=8, the volume ratio of the mixture to the sodium hydroxide aqueous solution is 1:2.5)" is changed to "continue stirring the mixture and slowly dropwise add deionized water (the volume ratio of the mixture to the deionized water is 1:2.5)".

[0054] Comparative Example 2

[0055] This comparative example provides a Ganoderma lucidum bitter melon chromium tablet, the preparation method of which is the same as that of Example 1, except that in step (3), "adding glacial acetic acid to the filtrate 1 to obtain a filtrate 1 with a pH of 5, and then adding anhydrous ethanol solution so that the ethanol content in the filtrate 1 is 80%" is changed to "adding anhydrous ethanol solution to the filtrate 1 so that the ethanol content in the filtrate 1 is 80%".

[0056] Comparative Example 3

[0057] This comparative example provides a Ganoderma lucidum bitter melon chromium tablet, the preparation method of which is the same as that of Example 1, except that the "1-butyl-3-methylimidazolium acetate ([Bmim][OAc])" in step (3) is replaced by "1-methyl-5-chloroimidazole hexafluorophosphate ([MClIm][PF6])".

[0058] Comparative Example 3 uses a hydrophobic ionic liquid. When the Ganoderma lucidum polysaccharide extract, the Momordica charantia extract and 1-methyl-5-chloroimidazole hexafluorophosphate are mixed, stratification occurs, resulting in a significant decrease in the extraction rate and purity.

[0059] The purity of the Ganoderma lucidum polysaccharides and momordicin obtained in Examples 1-3 and Comparative Examples 1-3 was tested and their extraction rates were calculated, wherein the Ganoderma lucidum polysaccharide extraction rate = (the final extracted Ganoderma lucidum polysaccharide mass / the Ganoderma lucidum mass) ×%, the momordicin extraction rate = (the final extracted momordicin mass / the momordicin mass) ×%, and the experimental results are shown in Table 1.

[0060] Table 1 Purity and extraction rate of Ganoderma lucidum polysaccharide and Momordica charantia in each embodiment and comparative example

[0061] sample Ganoderma lucidum polysaccharide purity Ganoderma lucidum polysaccharide extraction rate Purity of Momordica charantia Momordica charantia extraction rate Example 1 87％ 10.6％ 75％ 2.5％ Example 2 83％ 9.5％ 76％ 2.3％ Example 3 85％ 10.2％ 72％ 2.4％ Comparative Example 1 62％ 5.3％ 65％ 1.2％ Comparative Example 2 82％ 9.8％ 51％ 0.9％ Comparative Example 3 36％ 7.3％ 12％ 0.6％

[0062] In the present invention, it can be seen from Table 1 that the selection of ionic liquid and the control of conditions during the extraction process have a great influence on the purity and extraction rate of Ganoderma lucidum polysaccharide and momordicin.

[0063] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

Claims

1. A method for preparing Ganoderma lucidum and bitter melon chromium tablets, characterized in that: The steps include: S1. taking the supernatant of the bitter melon juice to obtain a bitter melon extract; S2, obtaining a Ganoderma lucidum extract by ultrasonic extraction; S3, adding an alkaline aqueous solution to the mixture of the bitter melon extract, the ganoderma lucidum extract and the imidazole acetate ionic liquid to obtain ganoderma lucidum polysaccharide and a filtrate; S4, adjusting the filtrate in step S3 to an acidic filtrate, adding anhydrous ethanol to the acidic filtrate to obtain momordica charantia; S5. Prepare tablets from ganoderma lucidum polysaccharide, momordica charantia, chromium picolinate, starch, sodium carboxymethyl starch, silicon dioxide and magnesium stearate.

2. The method for preparing the Ganoderma lucidum and bitter melon chromium tablets according to claim 1, characterized in that: In step S1, the supernatant of the bitter melon juice is obtained by filtering the bitter melon juice and then centrifuging it. The centrifugal speed is 6000-8000 rpm and the centrifugal time is 20-40 min.

3. The method for preparing the Ganoderma lucidum and bitter melon chromium tablets according to claim 1 or 2, characterized in that: In step S2, the ultrasonic extraction method has an ultrasonic power of 150-300 W, an ultrasonic frequency of 50-100 kHz, and an ultrasonic time of 2-5 h.

4. The method for preparing the Ganoderma lucidum bitter melon chromium tablets according to any one of claims 1 to 3, characterized in that: In step S3, the mass ratio of the bitter melon extract, the ganoderma lucidum extract and the imidazole acetate ionic liquid is 1:1:0.

5.

5. The method for preparing the Ganoderma lucidum bitter melon chromium tablets according to any one of claims 1 to 4, characterized in that: In step S3, the volume ratio of the mixture of the bitter melon extract, the ganoderma lucidum extract and the imidazole acetate ionic liquid to the alkaline aqueous solution is 1:2-3.

6. The method for preparing the Ganoderma lucidum bitter melon chromium tablets according to any one of claims 1 to 5, characterized in that: In step S3, the pH of the alkaline aqueous solution is 8; Preferably, the alkaline aqueous solution is prepared from sodium hydroxide and deionized water.

7. The method for preparing the Ganoderma lucidum bitter melon chromium tablets according to any one of claims 1 to 6, characterized in that: In step S4, the pH of the acidic filtrate is 5; Preferably, the filtrate in step S3 is adjusted to an acidic filtrate by acetic acid.

8. The method for preparing the Ganoderma lucidum bitter melon chromium tablets according to any one of claims 1 to 7, characterized in that: In step S4, the volume ratio of the acidic filtrate to anhydrous ethanol is 1:2.3-5.

9. The method for preparing the Ganoderma lucidum bitter melon chromium tablets according to any one of claims 1 to 8, characterized in that: The ganoderma lucidum polysaccharide and momordica charantia need to be subjected to reduced pressure distillation before being made into tablets.

10. A Ganoderma lucidum and bitter melon chromium tablet, which is prepared by the preparation method according to any one of claims 1 to 9.