Method for efficiently and synergistically extracting and preparing asparagine and polysaccharide

Abstract

The embodiment of the invention provides an efficient synergistic extraction preparation method of asparagine and polysaccharide, the utilization rate of raw materials and the extraction efficiency of components are improved, and the method comprises the following steps: S1, extracting asparagine: S11, cutting radix asparagi into segments; s12, an ethanol solution with the volume fraction being 60%-80% is added, the material-liquid ratio is 1: 10-1: 30 g / mL, and soaking is conducted for 30-60 min; s13, sealing, placing in a constant-temperature oscillator, oscillating and extracting at 50-70 DEG C for 60-90 minutes, and filtering to obtain an extracting solution; s14, performing vacuum concentration on the extracting solution; and S15, freeze-drying the concentrated solution to obtain an asparagine crude extract. S2, extracting radix asparagi polysaccharide, namely filtering in S21 and S13 to obtain filter residues; s22, volatilizing the ethanol solution on the surface of the filter residue; s23, distilled water is added, the material-liquid ratio is 1: 20-1: 40 g / mL, and soaking is conducted for 30-60 min; s24, placing in a Soxhlet extractor, carrying out reflux extraction at 70-100 DEG C for 60-90 minutes, and filtering to obtain an extracting solution; s25, performing vacuum concentration on the extracting solution; s26, centrifuging or filtering out precipitates, and combining the precipitates; and S27, freeze-drying the precipitate to obtain the radix asparagi polysaccharide extract.

Description

Technical Field

[0001] The present application relates to the technical field of asparagus processing, and in particular to a method for the efficient synergistic extraction and preparation of asparagus saponins and polysaccharides. Background Art

[0002] Asparagus cochinchinensis (Lour) Merr., the dried tuber of the Liliaceae plant, is a traditional Chinese medicine for tonifying yin, known for its moistening properties, lung nourishment, and fluid production. It was designated as a food-drug homologous substance in 2024. Rich in polysaccharides and saponins, asparagus has multiple effects, including antitussive and expectorant, antioxidant, anti-aging, anti-fatigue, and hypoglycemic properties.

[0003] In recent years, with the aggravation of the problem of population aging and the increase in the number of sub-healthy people, the field of health and wellness products has ushered in huge demand. Medicinal and edible substances have been favored and paid attention to due to their edibility and health value. However, when preparing related products, they often need to be added in the form of additives. Therefore, it is very necessary to extract and separate their components and prepare them into active products that can be added.

[0004] The yield of asparagus saponin in existing preparation methods is 1.5%-5.8%, and the yield of asparagus polysaccharide is 4.2%-14.7%. Most of them are extracted in the laboratory before conducting composition and pharmacological efficacy research. The utilization rate of raw materials is low and they are not suitable for production use. Summary of the Invention

[0005] The purpose of this application is to provide a highly efficient synergistic extraction and preparation method for asparagus saponin and polysaccharide, which improves the utilization rate of raw materials and the extraction efficiency of components and is suitable for production.

[0006] The present application solves the technical problem by adopting the following technical solutions.

[0007] The present invention provides a method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide, comprising the following steps:

[0008] S1, asparagus saponin extraction:

[0009] S11, cut the asparagus root into sections;

[0010] S12, adding 60% to 80% ethanol solution by volume, with a material-liquid ratio of 1:10 to 1:30 g / mL, and soaking for 30 to 60 minutes;

[0011] S13, after sealing, placing in a constant temperature oscillator, shaking extraction at 50-70°C for 60-90 minutes, and filtering to obtain the extract;

[0012] S14, vacuum concentrating the extract;

[0013] S15, freeze-drying the concentrated solution to obtain a crude asparagus saponin extract.

[0014] S2, Asparagus polysaccharide extraction:

[0015] S21, S13 are filtered to obtain filter residue;

[0016] S22, evaporating the ethanol solution on the surface of the filter residue;

[0017] S23, add distilled water with a solid-liquid ratio of 1:20 to 1:40 g / mL and soak for 30 to 60 minutes;

[0018] S24, placing the extract in a Soxhlet extractor, extracting under reflux at 70-100° C. for 60-90 min, and filtering to obtain an extract;

[0019] S25, vacuum concentrating the extract;

[0020] S26, adding 95% ethanol or anhydrous ethanol to the concentrate until the alcohol content reaches 80%, centrifuging or filtering to remove the precipitate, and combining the precipitates;

[0021] S27, freeze-drying the precipitate to obtain the asparagus polysaccharide extract.

[0022] Preferably, S13 is performed 1-3 times, and the extracts are filtered and combined.

[0023] Preferably, S24 is operated 1-3 times, and the extracts are filtered and combined.

[0024] Preferably, the vacuum concentration conditions in S14 are: concentration to 5-10% of the original volume at 40-60°C; and the vacuum concentration conditions in S25 are: concentration to 10-20% of the original volume at 50-70°C.

[0025] Preferably, the precipitate after centrifugation or filtration is dissolved in a small amount of hot water and step S26 is repeated once, and the precipitate is combined and entered into S27.

[0026] Preferably, in S26, the centrifugation condition is: centrifugation at 4000 rpm for 10 min.

[0027] Preferably, in S11, the asparagus root is cut into thin segments of 0.2 cm to 0.5 cm.

[0028] Preferably, in S22, an electric fan is used to accelerate volatilization.

[0029] Compared with the prior art, the embodiments of the present application have at least the following advantages or beneficial effects:

[0030] 1. Improved raw material utilization: Traditional methods often rely on extracting a single component from asparagus, resulting in low raw material utilization. This technology fully utilizes the asparagus raw material by extracting saponins first and then polysaccharides, avoiding resource waste.

[0031] 2. Improve extraction efficiency and yield: Optimized extraction conditions (such as appropriate ethanol concentration, material-liquid ratio, extraction temperature and time, etc.) can effectively promote the dissolution of saponins and polysaccharides, and can increase the yield of asparagus saponins and polysaccharides compared to existing technologies.

[0032] 3. The use of constant temperature oscillation to extract saponins and Soxhlet reflux to extract polysaccharides enhances the mass transfer effect during the extraction process and further improves the extraction efficiency: Constant temperature oscillation extraction maintains the stability of solvent solubility through constant temperature control. The oscillating action causes the raw material and solvent to continuously collide and mix, destroying the "static liquid film" on the surface of the raw material (a barrier that hinders mass transfer), allowing saponins to diffuse more quickly from the interior of the raw material particles into the solvent. This is equivalent to enhancing the mass transfer rate and uniformity through mechanical stirring and temperature control. The Soxhlet extractor uses solvent boiling to generate steam, which is then dripped into the raw material after condensation. After soaking the raw material, it is then refluxed through a siphon, forming an "extraction-reflux-reextraction" cycle. This method repeatedly allows the solvent to contact the raw material, continuously renewing the solvent concentration around the raw material and reducing the concentration difference resistance during the mass transfer process. This is equivalent to improving mass transfer efficiency through solvent circulation and long-term contact, allowing polysaccharides to dissolve more fully.

[0033] 4. Easy to operate and suitable for industrial production: The process steps are clear and the operation is relatively simple. The extraction conditions (such as temperature, time, ethanol concentration, etc.) are easy to control. The equipment used (such as constant temperature oscillator, Soxhlet extractor, vacuum concentrator, freeze dryer, etc.) are all common equipment in laboratories and industrial production, which is convenient for industrial promotion and application.

[0034] 5. Ensure product quality: Vacuum concentration is carried out at low temperature, which can reduce the degradation and destruction of saponins and polysaccharides during the concentration process, ensuring the active ingredient content of the product. Freeze drying is easy to use and can maintain the original structure and activity of the extract, avoid component denaturation caused by high-temperature drying, and improve product quality.

[0035] 6. Avoid using asparagus powder as raw material to overcome the shortcomings of asparagus's high polysaccharide and starch content, which makes it difficult to crush and unsuitable for production use. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the following is a brief introduction to the drawings required for use in the embodiments. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without creative work.

[0037] Figure 1 This is a flow chart of the efficient synergistic extraction and preparation method of asparagus saponin and polysaccharide provided in the examples of the present application. DETAILED DESCRIPTION

[0038] To make the purpose, technical solutions and advantages of the examples of the present application clearer, the technical solutions in the examples of the present application will be described clearly and completely below. Where specific conditions are not specified in the examples, conventional conditions or conditions recommended by the manufacturer are used. Where the manufacturer of the reagents or instruments is not specified, they are all conventional products that can be purchased commercially.

[0039] It should be noted that, in the absence of conflict, the embodiments and features of the embodiments in this application can be combined with each other. The present application will be described in detail below with reference to specific embodiments.

[0040] A method for efficiently synergistically extracting and preparing asparagus saponin and polysaccharide comprises the following steps:

[0041] S1, asparagus saponin extraction:

[0042] S11, cut the asparagus root into thin segments of 0.2 cm to 0.5 cm;

[0043] S12, adding 60% to 80% ethanol solution by volume, with a material-liquid ratio of 1:10 to 1:30 g / mL, and soaking for 30 to 60 minutes;

[0044] S13, after sealing, placing in a constant temperature oscillator, shaking extraction at 50-70°C for 60-90 minutes, and filtering to obtain the extract;

[0045] S14, vacuum concentrating the extract. Repeat S13 1-3 times, filter and combine the extracts; vacuum concentration conditions are: concentrating at 40-60°C to 5-10% of the original volume;

[0046] S15, freeze-drying the concentrated solution to obtain a crude asparagus saponin extract.

[0047] S2, Asparagus polysaccharide extraction:

[0048] S21, S13 are filtered to obtain filter residue;

[0049] S22, evaporate the ethanol solution on the surface of the filter residue. An electric fan can be used to accelerate the evaporation;

[0050] S23, add distilled water with a solid-liquid ratio of 1:20 to 1:40 g / mL and soak for 30 to 60 minutes;

[0051] S24, place in a Soxhlet extractor, extract under reflux at 70-100°C for 60-90 minutes, and filter to obtain an extract. Repeat S24 1-3 times, filter and combine the extracts;

[0052] S25, vacuum concentrating the extract. The vacuum concentration conditions are: concentrating to 10-20% of the original volume at 50-70°C;

[0053] S26, adding 95% ethanol or anhydrous ethanol to the concentrate until the alcohol content reaches 80%, centrifuging or filtering to remove the precipitate, and combining the precipitates. Centrifugation conditions are: centrifugation at 4000 rpm for 10 minutes. Dissolving the precipitate after centrifugation or filtration in a small amount of hot water, repeating step S26 once, combining the precipitates, and proceeding to S27;

[0054] S27, freeze-drying the precipitate to obtain the asparagus polysaccharide extract.

[0055] The principle behind this preparation method is that asparagus saponins are a highly polar steroidal saponin that is readily soluble in polar organic solvents such as ethanol. This technique exploits the high solubility of saponins in 60%-80% ethanol solutions. By soaking the asparagus, the ethanol is fully penetrated into the tissues of the asparagus. The mechanical forces of constant temperature oscillation disrupt the cellular structure, promoting the release of saponin components into the ethanol solution. Vacuum concentration reduces saponin loss due to high-temperature decomposition at low temperatures, while freeze-drying maintains the structural stability of the saponins, preventing denaturation during the drying process.

[0056] Asparagus polysaccharide is a polar macromolecular compound that is easily soluble in water. The polysaccharide component is retained in the filter residue after saponin extraction. By adding distilled water for soaking, the polysaccharide is fully swollen, and then reflux extraction is performed using a Soxhlet extractor at 70-100°C to further increase the dissolution rate of the polysaccharide. Adding high-concentration ethanol (95% ethanol or anhydrous ethanol) to the concentrate can reduce the solubility of the polysaccharide in the solution, causing it to precipitate. The precipitate is collected by centrifugation and freeze-dried to obtain a polysaccharide extract.

[0057] The features and performance of the present application are further described in detail below in conjunction with examples and comparative examples.

[0058]

[0059]

[0060] In summary, the extraction effect was optimal when the parameters of Example 2.2 were used. The optimized method achieved an overall yield of 8.2% for saponins, a 41.4% increase over the highest yield of the prior art. The optimized method also achieved an overall yield of 19.1% for polysaccharides, a 29.9% increase over the highest yield of the prior art.

[0061] This technology first uses ethanol to extract asparagus saponins, and then uses water to extract polysaccharides from the residue after extraction. This allows for the step-by-step extraction of two active ingredients from the same batch of asparagus raw materials, avoiding the mutual interference caused by the simultaneous extraction of multiple components in traditional methods, thereby improving the utilization rate of raw materials and the extraction efficiency of the components. By optimizing extraction conditions (such as ethanol concentration, material-liquid ratio, extraction temperature and time), the saponins and polysaccharides can achieve good dissolution effects during their respective extraction processes, thereby achieving efficient synergistic extraction.

[0062] The embodiments described above are part of the embodiments of the present application, rather than all of the embodiments. The detailed description of the embodiments of the present application is not intended to limit the scope of the present application for protection, but merely represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of this application.

Claims

1. A method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide, characterized in that: The following steps are involved: S1, asparagus saponin extraction: S11, cut the asparagus root into sections; S12, adding 60% to 80% ethanol solution by volume, with a material-liquid ratio of 1:10 to 1:30 g / mL, and soaking for 30 to 60 minutes; S13, after sealing, placing in a constant temperature oscillator, shaking extraction at 50-70°C for 60-90 minutes, and filtering to obtain the extract; S14, vacuum concentrating the extract; S15, freeze-drying the concentrated solution to obtain a crude asparagus saponin extract; S2, Asparagus polysaccharide extraction: S21, S13 are filtered to obtain filter residue; S22, evaporating the ethanol solution on the surface of the filter residue; S23, add distilled water with a solid-liquid ratio of 1:20 to 1:40 g / mL and soak for 30 to 60 minutes; S24, placing the extract in a Soxhlet extractor, extracting under reflux at 70-100° C. for 60-90 min, and filtering to obtain an extract; S25, vacuum concentrating the extract; S26, adding 95% ethanol or anhydrous ethanol to the concentrate until the alcohol content reaches 80%, centrifuging or filtering to remove the precipitate, and combining the precipitates; S27, freeze-drying the precipitate to obtain the asparagus polysaccharide extract.

2. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to claim 1, wherein: Repeat S13 for 1-3 times, and filter and combine the extracts.

3. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to claim 1, characterized in that: Perform S24 1-3 times, filter and combine the extracts.

4. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to claim 1, wherein: The vacuum concentration conditions in S14 are: concentration at 40-60° C. to 5-10% of the original volume; the vacuum concentration conditions in S25 are: concentration at 50-70° C. to 10-20% of the original volume.

5. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to claim 1, characterized in that: After centrifugation or filtration, the precipitate is dissolved in a small amount of hot water and step S26 is repeated once. The precipitate is combined and then proceeds to S27.

6. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to claim 1, characterized in that: In S26, the centrifugation condition is: centrifugation at 4000 rpm for 10 min.

7. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to any one of claims 1 to 6, characterized in that: In S11, the asparagus root is cut into thin segments of 0.2 cm to 0.5 cm.

8. The method for the efficient synergistic extraction and preparation of asparagus saponin and polysaccharide according to any one of claims 1 to 6, characterized in that: In S22, an electric fan is used to accelerate volatilization.

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