Rehmannia root extract and application thereof

Abstract

The present invention relates to the technical field of extraction of effective ingredients from traditional Chinese medicines, and proposes a Rehmannia glutinosa extract and its application. The preparation method comprises the following steps: S1, mixing Rehmannia glutinosa powder with a first extractant, heating for extraction, filtering, and concentrating to obtain a concentrated solution; the first extractant is a mixture of water and sodium dioctyl sulfosuccinate in a volume ratio of 97:3-99:1; S2, adding a second extractant to the concentrated solution, mixing evenly, standing for precipitation, centrifuging, collecting the precipitate, and drying to obtain a Rehmannia glutinosa extract; the second extractant comprises 80%-90% by mass of ethanol. Through the above technical solution, the problems of low polysaccharide content and low extraction rate in the Rehmannia glutinosa extract in the prior art are solved.

Description

Technical Field

[0001] The present invention relates to the technical field of extraction of effective components of traditional Chinese medicines, and in particular to a Rehmannia glutinosa extract and application thereof. Background Art

[0002] Rehmannia root (Shudihuang) is a processed root tuber from the Scrophulariaceae plant Rehmannia glutinosa. It has multiple pharmacological effects, including anti-aging, immune regulation, anti-tumor, memory enhancement, and antioxidant properties. Its chemical components include iridoid ether glycosides, amino acids, phenylethanoid glycosides, trace elements, polysaccharides, and ionones. Rehmannia root polysaccharides are the primary active ingredient in the herb, demonstrating immunity-boosting, anti-fatigue, and anti-anxiety properties.

[0003] Extracts containing Rehmannia glutinosa polysaccharides can be used in tobacco to enhance flavor, sweetness, promote salivation, and reduce irritation. Currently, water extraction and alcohol precipitation are the primary methods for extracting Rehmannia glutinosa extracts. However, this method results in a low extraction rate and low polysaccharide content, which limits its practical application. Therefore, developing a Rehmannia glutinosa extract with a high polysaccharide content is of great significance. Summary of the Invention

[0004] The present invention provides a Rehmannia root extract and application thereof, which solves the problems of low polysaccharide content and low extraction rate in the Rehmannia root extract in the related art.

[0005] The technical solutions of the present invention are as follows:

[0006] The present invention provides a Rehmannia glutinosa extract, the preparation method of which comprises the following steps:

[0007] S1. Mixing Rehmannia root powder with a first extractant, heating for extraction, filtering, and concentrating to obtain a concentrated solution;

[0008] The first extractant is a mixture of water and dioctyl sodium sulfosuccinate in a volume ratio of 97:3-99:1;

[0009] S2. Adding a second extractant to the concentrated solution, mixing uniformly, allowing to settle, centrifuging, collecting the precipitate, and drying to obtain a Rehmannia glutinosa extract;

[0010] The second extractant comprises 80%-90% by mass of ethanol.

[0011] As a further technical solution, in step S1, the solid-liquid ratio of the Rehmannia glutinosa powder to the first extractant is 1 g:20-30 mL.

[0012] As a further technical solution, in step S2, the volume ratio of the concentrated liquid to the second extractant is 1:4-6.

[0013] As a further technical solution, in step S1, the heating extraction is performed at a temperature of 70-80°C and for a time of 2-3 hours.

[0014] As a further technical solution, in step S2, the time for static precipitation is 24-36 hours.

[0015] As a further technical solution, in step S2, the second extractant further includes triethanolamine.

[0016] As a further technical solution, the volume ratio of ethanol to triethanolamine is 4-7:1.

[0017] As a further technical solution, the preparation method also includes post-extraction treatment: re-dissolving the Rehmannia root extract in water, adding an extractant, extracting and standing to separate the phases, removing the phase and ultrafiltration to obtain the retentate, concentrating, and freeze-drying to obtain the refined Rehmannia root extract.

[0018] As a further technical solution, during the concentration, the concentration is performed to a relative density of 1.14-1.17.

[0019] As a further technical solution, the extractant is formed by mixing polyethylene glycol and ammonium benzoate solution in a volume ratio of 1:1.

[0020] As a further technical solution, the molecular weight of the polyethylene glycol is 1500, the mass fraction is 14%-16%, and the mass fraction of the ammonium benzoate solution is 18%-20%.

[0021] The invention also proposes application of the Rehmannia glutinosa extract in cigarettes.

[0022] The working principle and beneficial effects of the present invention are:

[0023] 1. In the present invention, using a mixture of water and sodium dioctyl sulfosuccinate as the first extractant can increase the content of the Rehmannia root extract, improve the extraction efficiency, and increase the polysaccharide content in the extract. Using an ethanol solution as the second extractant can increase the extraction rate and the polysaccharide content in the extract, thereby solving the problem of low polysaccharide content in the Rehmannia root extract.

[0024] 2. In the present invention, the second extractant further includes triethanolamine. The addition of triethanolamine helps to improve the extraction capacity of the second extractant, thereby further increasing the extraction rate and the content of polysaccharides in the extract. When the volume ratio of ethanol to triethanolamine in the second extractant is 4-9:1, the extraction rate and the content of polysaccharides in the extract can be further improved.

[0025] 3. In the present invention, the preparation method of Rehmannia glutinosa extract further includes post-extraction treatment, which is conducive to increasing the content of polysaccharides in the extract. When the extractant is a mixed solution of polyethylene glycol and ammonium benzoate, it helps to further increase the content of polysaccharides in the extract. DETAILED DESCRIPTION

[0026] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0027] Example 1

[0028] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0029] S1. Mix 100 g of Rehmannia root powder with 990 mL of water and 10 mL of dioctyl sodium sulfosuccinate, heat and extract at 70°C for 3 h, filter, and concentrate to obtain 200 mL of concentrate;

[0030] S2. Add 600 mL of 80% ethanol by mass to the concentrated solution, mix well, let stand for 24 hours, centrifuge, collect the precipitate, and dry to obtain 22.7 g of Rehmannia glutinosa extract.

[0031] Example 2

[0032] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0033] S1. Mix 100 g of Rehmannia root powder with 3880 mL of water and 120 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0034] S2. Add 1400 mL of 90% ethanol by mass to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 24.8 g of Rehmannia glutinosa extract.

[0035] Example 3

[0036] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0037] S1. Mix 100 g of Rehmannia root powder with 1940 mL of water and 60 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0038] S2. Add 1400 mL of 90% ethanol by mass to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 24.6 g of Rehmannia glutinosa extract.

[0039] Example 4

[0040] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0041] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0042] S2. Add 1400 mL of 90% ethanol by mass to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 24.7 g of Rehmannia glutinosa extract.

[0043] Example 5

[0044] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0045] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0046] S2. Add 800 mL of 90% ethanol by mass to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 25.9 g of Rehmannia glutinosa extract.

[0047] Example 6

[0048] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0049] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0050] S2. Add 1200 mL of 90% ethanol by mass to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 25.4 g of Rehmannia glutinosa extract.

[0051] Example 7

[0052] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0053] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0054] S2. Add 600 mL of 90% ethanol and 200 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 27.1 g of Rehmannia glutinosa extract.

[0055] Example 8

[0056] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0057] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0058] S2. Add 720 mL of 90% ethanol and 80 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 27.3 g of Rehmannia glutinosa extract.

[0059] Example 9

[0060] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0061] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0062] S2. Add 640 mL of 90% ethanol and 160 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 27.6 g of Rehmannia glutinosa extract.

[0063] Example 10

[0064] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0065] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0066] S2. Add 700 mL of 90% ethanol and 100 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, collect the precipitate, and dry to obtain 27.8 g of Rehmannia glutinosa extract.

[0067] Example 11

[0068] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0069] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0070] S2. Add 700 mL of 90% ethanol and 100 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, and collect the precipitate to obtain 27.8 g of Rehmannia glutinosa extract;

[0071] S3. Redissolve the Rehmannia root extract in 2000 mL of water, add 500 mL of 14% by mass polyethylene glycol (molecular weight 1500) and 500 mL of 18% by mass ammonium sulfate solution, extract, let stand for phase separation, remove the lower phase and ultrafilter to obtain the retentate, concentrate to a relative density of 1.14, and freeze-dry to obtain the refined Rehmannia root extract.

[0072] Example 12

[0073] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0074] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0075] S2. Add 700 mL of 90% ethanol and 100 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, and collect the precipitate to obtain 27.8 g of Rehmannia glutinosa extract;

[0076] S3. Redissolve the Rehmannia root extract in 2000 mL of water, add 500 mL of 14% by mass polyethylene glycol (molecular weight 1500) and 500 mL of 18% by mass ammonium benzoate solution, extract, let stand for phase separation, remove the lower phase and ultrafilter to obtain the retentate, concentrate to a relative density of 1.14, and freeze-dry to obtain the refined Rehmannia root extract.

[0077] Example 13

[0078] A preparation method of Rehmannia glutinosa extract comprises the following steps:

[0079] S1. Mix 100 g of Rehmannia root powder with 2910 mL of water and 90 mL of dioctyl sodium sulfosuccinate, heat and extract at 80°C for 2 h, filter, and concentrate to obtain 200 mL of concentrated solution;

[0080] S2. Add 700 mL of 90% ethanol and 100 mL of triethanolamine to the concentrated solution, mix well, let stand for 36 hours, centrifuge, and collect the precipitate to obtain 27.8 g of Rehmannia glutinosa extract;

[0081] S3. Redissolve the Rehmannia root extract in 2000 mL of water, add 500 mL of 16% by mass polyethylene glycol (molecular weight 1500) and 500 mL of 20% by mass ammonium benzoate solution, extract, let stand for phase separation, remove the lower phase and ultrafilter to obtain the retentate, concentrate to a relative density of 1.17, and freeze-dry to obtain the refined Rehmannia root extract.

[0082] Comparative Example 1

[0083] The only difference between this comparative example and Example 1 is that no sodium dioctyl sulfosuccinate was added in step S1 of this comparative example, and the volume of water was 1000 mL.

[0084] The following measurements were performed on the Rehmannia glutinosa extracts prepared in Examples 1-10 and Comparative Example 1:

[0085] ① Extraction rate: Calculate the extraction rate of Rehmannia root extract according to the following formula:

[0086] Extraction rate (%) = (mass of Rehmannia root extract / mass of Rehmannia root powder) × 100;

[0087] ②Polysaccharide content: Using glucose as the standard, the phenol-sulfuric acid method was adopted, and the absorbance was measured at 490 nm using a 721 spectrophotometer. The regression equation Y=0.007083X+0.0092 (r=0.9987) was established to determine the polysaccharide content in the Rehmannia glutinosa extract.

[0088] The measurement results are shown in Table 1 below.

[0089] Table 1 Extraction rate of Rehmannia glutinosa extract and content of polysaccharide in the extract of Examples 1-10 and Comparative Example 1

[0090]

[0091] It can be seen from the data in the table that the preparation method of the present invention has a high extraction rate, and the prepared Rehmannia glutinosa extract has a high polysaccharide content. Comparison of Example 2 with Example 3-4 shows that the optimal range of the solid-liquid ratio of Rehmannia glutinosa powder to the first extractant is 1g:20-30mL. Comparison of Example 4 with Example 5-6 shows that the optimal volume ratio of the concentrate to the second extractant is 1:4-6. Comparison of Example 5 with Example 7-10 shows that the addition of triethanolamine to the second extractant is beneficial to further increase the extraction rate of Rehmannia glutinosa extract and the content of polysaccharides in the extract. Comparison of Example 1 with Comparative Example 1 shows that using a mixture of water and sodium dioctyl sulfosuccinate as the first extractant can increase the content of Rehmannia glutinosa extract, improve the extraction efficiency, and increase the content of polysaccharides in the extract.

[0092] The polysaccharide content of the Rehmannia root extract prepared in Example 10 and the refined Rehmannia root extract prepared in Examples 11-13 was determined. Glucose was used as the standard, the phenol-sulfuric acid method was adopted, and the absorbance was measured at 490 nm using a 721 spectrophotometer. The regression equation Y = 0.007083X + 0.0092 (r = 0.9987) was established to determine the polysaccharide content. The measurement results are shown in Table 2 below.

[0093] Table 2 Polysaccharide content in Examples 10-13

[0094]

[0095] As shown in Table 2, post-extraction treatment is beneficial for increasing the content of polysaccharide compounds in the Rehmannia glutinosa extract. Comparison between Example 11 and Example 12 shows that using a mixed solution of polyethylene glycol and ammonium benzoate as an extractant can further increase the content of polysaccharides in the Rehmannia glutinosa extract compared to using a mixed solution of polyethylene glycol and ammonium sulfate as an extractant.

[0096] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A Rehmannia root extract, characterized in that The preparation method comprises the following steps: S1. Mixing Rehmannia root powder with a first extractant, heating for extraction, filtering, and concentrating to obtain a concentrated solution; The first extractant is a mixture of water and dioctyl sodium sulfosuccinate in a volume ratio of 97:3-99:1; S2. Adding a second extractant to the concentrated solution, mixing uniformly, allowing to settle, centrifuging, collecting the precipitate, and drying to obtain a Rehmannia glutinosa extract; The second extractant comprises 80% to 90% by mass of ethanol; The second extractant further comprises triethanolamine, and the volume ratio of the ethanol to triethanolamine is 4-7:1; In step S2, the volume ratio of the concentrated liquid to the second extractant is 1:4-6.

2. The Rehmannia glutinosa extract according to claim 1, wherein In step S1, the solid-liquid ratio of the Rehmannia glutinosa powder to the first extractant is 1 g:20-30 mL.

3. The Rehmannia root extract according to claim 1, wherein In step S1, the heating extraction is performed at a temperature of 70-80° C. and a time of 2-3 hours.

4. The Rehmannia root extract according to claim 1, characterized in that In step S2, the time for the static precipitation is 24-36 hours.

5. The Rehmannia glutinosa extract according to claim 1, characterized in that The preparation method also includes post-extraction treatment: re-dissolving the Radix Rehmanniae Preparata extract with water, adding an extractant, extracting and standing to separate phases, removing the phase and ultrafiltration to obtain a retentate, concentrating, and freeze-drying to obtain a refined Radix Rehmanniae Preparata extract.

6. The Rehmannia root extract according to claim 5, characterized in that The extractant is prepared by mixing polyethylene glycol and ammonium benzoate solution in a volume ratio of 1:

1.

7. The Rehmannia root extract according to claim 6, characterized in that The molecular weight of the polyethylene glycol is 1500, and the mass fraction is 14%-16%. The mass fraction of the ammonium benzoate solution is 18%-20%.

8. Use of the Rehmannia glutinosa extract according to any one of claims 1 to 7 in cigarettes.

Images