Longevity tonic and preparation method thereof
By introducing a self-developed stabilizer into the Longevity Tonic Juice, and using anhydride-modified starch, chitosan, and biopowder to construct an interfacial film, the problem of easy volatility and oxidation of volatile oils was solved, thereby improving the stability and bioavailability of the product and ensuring the antioxidant and aroma preservation of volatile oils and the sustained release of active ingredients.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIANGXI JINDING PHARM CO LTD
- Filing Date
- 2026-04-21
- Publication Date
- 2026-06-05
AI Technical Summary
In the existing production process of Longevity Tonic Juice, the volatile oils are prone to volatilization and oxidation, which leads to weakened aroma, unstable release of active ingredients, and affected efficacy. Furthermore, traditional processes are difficult to achieve antioxidant preservation of volatile oils and slow release of ingredients.
A self-developed stabilizer is used to synergistically construct an interfacial film with anhydride-modified starch, chitosan, and bio-powder to form a Pickering emulsion, which inhibits the thermal degradation and oxidation of volatile oils and delays release through particle anchoring.
It significantly improves the product stability and bioavailability of Longevity Tonic Juice, extends shelf life, ensures the antioxidant and aroma preservation of volatile oils and the sustained release of active ingredients, and enhances clinical efficacy.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of traditional Chinese medicine technology, and in particular to a longevity tonic juice and its preparation method. Background Technology
[0002] Longevity Tonic Juice is a traditional Chinese medicine compound preparation composed of thirteen medicinal herbs, including yam, codonopsis, angelica, and cinnamon twig. It is believed to invigorate qi and blood, regulate the spleen and stomach, and is widely used as an adjunct treatment for the elderly, those recovering from illness, and those with chronic fatigue syndrome. Current industrial production generally employs a decoction, alcohol precipitation, concentration, and bottling process: the herbs are decocted together, the decoction is precipitated with high-concentration ethanol to remove impurities, the ethanol is recovered, and excipients are added to adjust the volume. While this process is simple and easy to control, it still has significant drawbacks.
[0003] Volatile oils are key components for warming and invigorating the meridians and promoting blood circulation. However, due to their small molecular weight and low polarity, they are highly susceptible to volatilization, oxidation, or thermal degradation under conditions of high-temperature concentration, long-term storage, and light exposure. This leads to a weakening of the product's aroma and a decrease in its content, affecting clinical efficacy. Traditional compound preparations are true solutions or suspensions, where key indicator components such as paeoniflorin and glycyrrhizic acid are rapidly released in the early gastrointestinal tract, resulting in high peak concentrations but short durations of action, which is not conducive to sustained absorption of the drug's effects by debilitated patients.
[0004] For example, Chinese patent application CN116832137A discloses a longevity tonic juice suitable for diabetes patients, which invigorates qi, nourishes blood, and strengthens the spleen, along with its preparation process. Attempts have been made to encapsulate volatile oils using liposomes or nanoemulsions, but these methods involve long preparation routes, significant risks of organic solvent residue, and complex traditional Chinese medicine formulas, which can lead to problems such as low encapsulation rates, wide particle size distributions, and poor compatibility with decoctions, making direct application on oral liquid filling lines difficult.
[0005] Therefore, how to achieve the goals of antioxidant preservation of volatile oils, slow release of indicator components, and improved storage stability while maintaining the compatibility of the original process has become a technical bottleneck that urgently needs to be overcome in the modernization of Shouxing Tonic Juice. Summary of the Invention
[0006] To address the shortcomings of existing technologies, this invention aims to provide a longevity tonic juice and its preparation method that significantly improves product stability, bioavailability, and industrial adaptability by introducing novel stabilizers.
[0007] To achieve the above-mentioned objectives, the present invention adopts the following technical solution:
[0008] The preparation method of a longevity tonic is as follows:
[0009] The volatile oil and distillate of Angelica sinensis, cinnamon twig, and dried ginger are extracted by steam distillation and separated for later use. The residue is decocted with yam, stir-fried hawthorn, processed Polygonum multiflorum, Codonopsis pilosula, Poria cocos, stir-fried Atractylodes macrocephala, honey-processed licorice, stir-fried white peony root, Ophiopogon japonicus, and Rehmannia glutinosa. The decoction is filtered and concentrated. After alcohol precipitation, the ethanol is recovered and concentrated again. Sodium benzoate, stabilizer, polysorbate 80, the aforementioned volatile oil and distillate are added, stirred well and diluted to volume, and then bottled to obtain the final product.
[0010] The stabilizer is prepared by enzymatic hydrolysis of wheat starch with a compound enzyme, ultrasonic-assisted esterification modification with an acid anhydride compound, blending it with chitosan and biological powder, and then centrifuging, drying and sieving.
[0011] A further preferred embodiment of the preparation method for the Longevity Tonic is as follows:
[0012] This product is composed of 13 Chinese medicinal herbs, with the following specific ingredients and dosages: 200-280g of Chinese yam, 100-140g of stir-fried hawthorn, 100-140g of prepared Polygonum multiflorum, 180-220g of Codonopsis pilosula, 30-50g of Poria cocos, 20-30g of dried ginger, 70-90g of Angelica sinensis, 70-90g of cinnamon twig, 40-60g of stir-fried Atractylodes macrocephala, 40-60g of honey-processed licorice root, 40-60g of stir-fried white peony root, 40-60g of Ophiopogon japonicus, and 80-120g of prepared Rehmannia glutinosa.
[0013] First, take Angelica sinensis, Cinnamomum cassia, and Zingiber officinale, and extract their volatile oil components using steam distillation. Separate the oil-water mixture produced during distillation, collecting the volatile oil and the distilled aqueous solution separately in dedicated containers. Add water to the remaining medicinal residue after volatile oil extraction and decoct twice with the other ten medicinal materials in the prescription. Combine the two decoctions, filter, and concentrate to 550-700 mL. Add 1.5-3 times the volume of anhydrous ethanol to the concentrate, stir to precipitate impurities, let stand, filter, recover the ethanol from the filtrate, dilute with 400-800g of water, filter again, and concentrate to 300-400 mL. Add 1-5g of sodium benzoate, along with the aforementioned distilled aqueous solution and its volatile oil, 1-5g of stabilizer, and 1-10g of polysorbate 80. Adjust the total volume to 1000 mL with water, stir well, and bottle to obtain the Longevity Tonic Juice.
[0014] The first addition of water for decoction involves adding 10-15L of water and decocting for 2-6 hours.
[0015] The second addition of water involves adding 5-10L of water and simmering for 1-5 hours.
[0016] A further preferred embodiment is the method for preparing the stabilizer as follows:
[0017] S1. Mix 20-50g wheat starch, 0.8-1.5g compound enzyme, and 300-500g phosphate buffer in a shaker at 100-300rpm and 40-45℃ for 2-6 hours. Adjust the pH to 6.5-7.5 with 0.05-0.2mol / L NaOH aqueous solution. Centrifuge at 3000-5000rpm for 0.5-3 minutes and dry at 30-45℃ for 5-12 hours to obtain enzymatically hydrolyzed starch.
[0018] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 30-40℃ for 10-30 minutes to prepare a 5-15wt% mixture, and adjust the pH to 9-10.5 with 0.05-0.2mol / L NaOH aqueous solution; mix 1-3g of acid anhydride compound with 2-6g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate after each addition. After each sonication, adjust the pH to 9-10.5 again with 0.05-0.2mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 10-30 minutes, adjust the pH to 6-6.8 with 0.05-0.2mol / L hydrochloric acid, centrifuge at 3000-5000rpm for 5-15 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 30-45℃ for 5-20 hours, and pass through a 100-300 mesh sieve to obtain modified starch;
[0019] S3. Prepare a 3-8 wt% mixture by adding modified starch to water; add 2-6 g of chitosan to 200-400 g of 1-3 wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 0.5-2 g of biological powder to 40-60 g of water and stir evenly to obtain a biological powder liquid; mix the above three liquids, stir at 300-800 rpm for 10-50 minutes, centrifuge at 3000-5000 rpm for 5-15 minutes, collect the precipitate, dry at 30-45℃ for 5-20 hours, and pass through a 100-300 mesh sieve to obtain the stabilizer.
[0020] The complex enzyme is composed of α-amylase, β-amylase, and pullulanase mixed in a mass ratio of 0.5-2:0.5-2:1-3.
[0021] In step S2, the ultrasonic treatment power is 200-600W and the time is 5-10 minutes.
[0022] The acid anhydride compound is at least one of dodecenyl succinic anhydride and hexadecenyl succinic anhydride.
[0023] The biological powder is at least one of buffalo horn powder, mother-of-pearl powder, and gastrodia elata powder.
[0024] Longevity Tonic Juice is composed of 13 Chinese medicinal herbs, each playing a specific role in the formula. These herbs work synergistically to achieve the overall effect of invigorating qi and nourishing blood, strengthening the spleen and stomach. The functions of each herb are as follows:
[0025] Yam: It nourishes the spleen and stomach, promotes the production of body fluids and benefits the lungs, tonifies the kidneys and astringes essence, and enhances the body's immunity.
[0026] Stir-fried hawthorn: It helps with digestion, promotes qi circulation, and improves blood circulation.
[0027] Prepared Polygonum multiflorum: Nourishes essence and blood, strengthens the kidneys and darkens hair; used for blood deficiency with chlorosis, dizziness and insomnia.
[0028] Codonopsis pilosula: replenishes qi and strengthens the spleen and lungs, enhances physical strength and improves fatigue.
[0029] Poria cocos: promotes diuresis and eliminates dampness, strengthens the spleen and calms the mind, promotes fluid metabolism and soothes the nerves.
[0030] Dried ginger: warms the middle jiao and dispels cold, restores yang and unblocks the meridians, warms the spleen and stomach and relieves cold symptoms.
[0031] Angelica sinensis: Nourishes and invigorates blood, regulates menstruation and relieves pain, moistens the intestines and promotes bowel movement, and improves blood deficiency and pain.
[0032] Cinnamon twig: It induces sweating and relieves muscle tension, warms and unblocks the meridians, assists yang and transforms qi, and promotes blood circulation.
[0033] Stir-fried Atractylodes macrocephala: It strengthens the spleen and replenishes qi, dries dampness and promotes diuresis, stops sweating and calms the fetus, and enhances digestive function.
[0034] Honey-processed licorice: Tonifies the spleen and stomach, replenishes qi and restores pulse, harmonizes other medicines, and alleviates toxicity.
[0035] Stir-fried white peony root: nourishes blood and astringes yin, softens the liver and relieves pain, calms liver yang, and relieves muscle spasms.
[0036] Ophiopogon japonicus: Nourishes Yin and generates fluids, moistens the lungs and clears the heart, relieves dryness and cough.
[0037] Rehmannia glutinosa (processed): Nourishes Yin and blood, replenishes essence and marrow, and is used for blood deficiency and kidney deficiency syndromes.
[0038] Sodium benzoate acts as a preservative, inhibiting microbial growth and extending product shelf life.
[0039] Polysorbate 80, as a nonionic surfactant, reduces interfacial tension and improves emulsification uniformity and stability.
[0040] Stabilizers are used to enhance the emulsification stability and shelf life of Shouxing Tonic Juice. The following are the roles of key substances in its preparation process:
[0041] Wheat starch serves as a matrix material, providing a carbohydrate base, and its adsorption and stability are enhanced through modification.
[0042] Complex enzymes (α-amylase, β-amylase, pullulanase) act as enzymatic hydrolysants for starch granules, disrupting the crystal structure, increasing porosity, and enhancing reactivity.
[0043] Dodecenyl succinic anhydride, as a hydrophobic agent, is esterified with starch hydroxyl groups to introduce carboxyl groups, thereby enhancing emulsification and interfacial activity.
[0044] Chitosan, as a cationic polysaccharide, binds to modified starch through electrostatic interactions to form a stable complex, thereby improving the mechanical strength of the particles.
[0045] Mother-of-pearl powder provides a mineral matrix, enhances adsorption capacity, improves hydrophobicity, and helps stabilize the oil-water interface.
[0046] Anhydrous ethanol is used as a solvent and detergent to dilute and purify reaction products and remove impurities.
[0047] Citric acid is used to prepare acidic solutions, promote the dissolution of chitosan, and provide a protonated environment.
[0048] Hydrochloric acid is used to adjust the pH value, neutralize alkaline conditions, and terminate the esterification reaction.
[0049] NaOH adjusts the pH value, creating an alkaline environment that promotes esterification and electrostatic bonding.
[0050] Phosphate buffer maintains a stable pH environment for the enzymatic hydrolysis reaction, ensuring enzyme activity.
[0051] Compared with the prior art, the present invention has the following beneficial technical effects:
[0052] 1) This invention introduces a self-developed stabilizer into the Longevity Tonic Juice. By synergistically constructing an interfacial film with anhydride-modified starch, chitosan, and biological powder, it significantly inhibits the thermal degradation and oxidation of volatile oils and extends the product's shelf life.
[0053] 2) The stabilizer particles of the present invention can anchor the oil-water interface to form a Pickering emulsion, delay the release rate of volatile oils, improve the delivery efficiency of active components in the gastrointestinal tract, and enhance bioavailability.
[0054] 3) The functions and indications of the Longevity Tonic Juice of this invention are to invigorate qi and nourish blood, and regulate the spleen and stomach. It is effective for elderly people who are weak, recovering from illness, fatigue, loss of appetite, limb pain and numbness, insomnia and dreaminess. Detailed Implementation
[0055] Some material parameters and their sources:
[0056] Yam, a commercially available product, originating from Jiaozuo City, Henan Province.
[0057] Roasted hawthorn, a commercially available product, originating from Xinglong Mountain, Hebei Province.
[0058] Processed Polygonum multiflorum, a commercially available product, originating from southeastern Guizhou.
[0059] Codonopsis pilosula, a commercially available product, originates from Changzhi, Shanxi Province.
[0060] Poria cocos, a commercially available product, originates from Jingzhou County, Huaihua City, Hunan Province.
[0061] Dried ginger, a commercially available product, originating from Qianwei, Sichuan.
[0062] Angelica sinensis, a commercially available product, originates from Minxian County, Gansu Province.
[0063] Cinnamon twigs, a commercially available product, originating from Luoding, Guangdong.
[0064] Stir-fried Atractylodes macrocephala, a commercially available product, originating from Yuqian, Zhejiang.
[0065] Honey-processed licorice root, a commercially available product, originating from Minqin County, Gansu Province.
[0066] Fried white peony root, a commercially available product, originating from Luoyang, Henan Province.
[0067] Ophiopogon japonicus, a commercially available product, originates from Santai County, Mianyang City, Sichuan Province.
[0068] Rehmannia glutinosa (processed), a commercially available product, originates from Jiaozuo, Henan Province.
[0069] Wheat starch, product grade: food grade, item number: 1004, Jinan Yufuyuan Biotechnology Co., Ltd.
[0070] Phosphate buffer, pH=5.8, concentration: 0.2mol / L.
[0071] α-Amylase, enzyme activity: 20,000 u / g.
[0072] β-Amylase, enzyme activity: 700,000 u / g.
[0073] Pullulanase, enzyme activity: 100,000 u / g.
[0074] Chitosan, Product No.: BR-024, Grade: Food Grade, Henan Bangrun Chemical Products Co., Ltd.
[0075] Pearl powder, particle size: 80-120 mesh, Ningxia Xiangcao Biotechnology Co., Ltd.
[0076] Gastrodia elata powder, product number: HY-8952585, product grade: food grade, manufactured by Xi'an Haoyu Kangze Biotechnology Co., Ltd.
[0077] Buffalo horn powder, product number: SH-392, product grade: food grade, Shaanxi Sihai Biotechnology Co., Ltd.
[0078] Earthworm protein powder, grade: food grade, item number: tb-0625-064, Tianben Biotechnology (Shanxi) Co., Ltd.
[0079] All other raw materials used in the embodiments and comparative examples of this invention are commercially available products.
[0080] Example 1
[0081] The preparation method of a longevity tonic is as follows:
[0082] This product is composed of 13 Chinese medicinal herbs, and the specific ingredients and dosages are as follows: 240g of Chinese yam, 120g of stir-fried hawthorn, 120g of prepared Polygonum multiflorum, 200g of Codonopsis pilosula, 40g of Poria cocos, 25g of dried ginger, 80g of Angelica sinensis, 80g of cinnamon twig, 50g of stir-fried Atractylodes macrocephala, 50g of honey-processed licorice, 50g of stir-fried white peony root, 50g of Ophiopogon japonicus, and 100g of prepared Rehmannia glutinosa.
[0083] First, take three medicinal herbs: Angelica sinensis, Cinnamomum cassia, and Zingiber officinale. Slice them to a particle size of less than 3 mm. Place the herbs in a distillation flask and steam distill for 4 hours. Transfer the distillate to a separatory funnel and let it stand for 50 minutes to allow for natural separation. Open the stopcock of the separatory funnel and collect the aqueous solution and volatile oil separately for later use. Add the remaining herb residue after extracting the volatile oil to the remaining ten herbs in the prescription and decoct twice. For the first decoction, add 12.5 L of water and decoct for 4 hours. For the second decoction, add 7.5 L of water and decoct for 2 hours. Hours; combine the two decoctions, filter and concentrate to 620mL, add 2 times the volume of anhydrous ethanol to the above concentrate, stir to precipitate impurities, let stand and filter, treat the filtrate with recovered ethanol, add 600g of water to dilute, filter again and concentrate to 350mL; add 1g of sodium benzoate, and at the same time add the aforementioned distilled aqueous solution and its volatile oil, then add 3g of stabilizer and 5g of polysorbate 80, add water to adjust the total volume to 1000mL, stir well, fill into bottles, and the longevity tonic juice is obtained.
[0084] The stabilizer is prepared as follows:
[0085] S1. 40g wheat starch, 1.2g compound enzyme, and 400g phosphate buffer were treated on a shaker at 150rpm and 42℃ for 4 hours. The pH was adjusted to 7.0 with 0.1mol / L NaOH aqueous solution. The mixture was centrifuged at 4000rpm for 1 minute and dried at 40℃ for 10 hours to obtain enzymatically hydrolyzed starch. The compound enzyme was a mixture of α-amylase, β-amylase, and pullulanase in a mass ratio of 1:1:2.
[0086] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 35°C for 20 minutes to prepare a 10wt% mixture, and adjust the pH to 10 with 0.1mol / L NaOH aqueous solution; mix 2g of dodecenyl succinic anhydride with 4g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate at 400W for 8 minutes after each addition of treatment agent. After each sonication, adjust the pH to 10 again with 0.1mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 20 minutes, adjust the pH to 6.5 with 0.1mol / L hydrochloric acid, centrifuge at 4000rpm for 10 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 40°C for 12 hours, and pass through a 150-mesh sieve to obtain modified starch;
[0087] S3. Prepare a 5wt% mixture by adding modified starch to water; add 4g of chitosan to 300g of 2wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 1g of pearl powder to 50g of water and stir evenly to obtain a pearl powder solution; mix the above three liquids, stir at 500rpm for 30 minutes, centrifuge at 4000rpm for 10 minutes, collect the precipitate, dry at 40℃ for 12 hours, and pass through a 150-mesh sieve to obtain the stabilizer.
[0088] Example 2
[0089] The preparation method of the longevity tonic juice is basically the same as that in Example 1, except that the preparation method of the stabilizer is different.
[0090] The stabilizer is prepared as follows:
[0091] S1. 40g wheat starch, 1.2g compound enzyme, and 400g phosphate buffer were treated on a shaker at 150rpm and 42℃ for 4 hours. The pH was adjusted to 7.0 with 0.1mol / L NaOH aqueous solution. The mixture was centrifuged at 4000rpm for 1 minute and dried at 40℃ for 10 hours to obtain enzymatically hydrolyzed starch. The compound enzyme was a mixture of α-amylase, β-amylase, and pullulanase in a mass ratio of 1:1:2.
[0092] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 35°C for 20 minutes to prepare a 10wt% mixture, and adjust the pH to 10 with 0.1mol / L NaOH aqueous solution; mix 2g of hexadecenyl succinic anhydride with 4g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate at 400W for 8 minutes after each addition of treatment agent. After each sonication, adjust the pH to 10 again with 0.1mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 20 minutes, adjust the pH to 6.5 with 0.1mol / L hydrochloric acid, centrifuge at 4000rpm for 10 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 40°C for 12 hours, and pass through a 150-mesh sieve to obtain modified starch;
[0093] S3. Prepare a 5wt% mixture by adding modified starch to water; add 4g of chitosan to 300g of 2wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 1g of pearl powder to 50g of water and stir evenly to obtain a pearl powder solution; mix the above three liquids, stir at 500rpm for 30 minutes, centrifuge at 4000rpm for 10 minutes, collect the precipitate, dry at 40℃ for 12 hours, and pass through a 150-mesh sieve to obtain the stabilizer.
[0094] Example 3
[0095] The preparation method of the longevity tonic juice is basically the same as that in Example 1, except that the preparation method of the stabilizer is different.
[0096] The stabilizer is prepared as follows:
[0097] S1. 40g wheat starch, 1.2g compound enzyme, and 400g phosphate buffer were treated on a shaker at 150rpm and 42℃ for 4 hours. The pH was adjusted to 7.0 with 0.1mol / L NaOH aqueous solution. The mixture was centrifuged at 4000rpm for 1 minute and dried at 40℃ for 10 hours to obtain enzymatically hydrolyzed starch. The compound enzyme was a mixture of α-amylase, β-amylase, and pullulanase in a mass ratio of 1:1:2.
[0098] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 35°C for 20 minutes to prepare a 10wt% mixture, and adjust the pH to 10 with 0.1mol / L NaOH aqueous solution; mix 2g of dodecenyl succinic anhydride with 4g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate at 400W for 8 minutes after each addition of treatment agent. After each sonication, adjust the pH to 10 again with 0.1mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 20 minutes, adjust the pH to 6.5 with 0.1mol / L hydrochloric acid, centrifuge at 4000rpm for 10 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 40°C for 12 hours, and pass through a 150-mesh sieve to obtain modified starch;
[0099] S3. Prepare a 5wt% mixture by adding modified starch to water; add 4g of chitosan to 300g of 2wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 1g of Gastrodia elata powder to 50g of water and stir evenly to obtain Gastrodia elata powder solution; mix the above three liquids, stir at 500rpm for 30 minutes, centrifuge at 4000rpm for 10 minutes, collect the precipitate, dry at 40℃ for 12 hours, and pass through a 150-mesh sieve to obtain the stabilizer.
[0100] Example 4
[0101] The preparation method of the longevity tonic juice is basically the same as that in Example 1, except that the preparation method of the stabilizer is different.
[0102] The stabilizer is prepared as follows:
[0103] S1. 40g wheat starch, 1.2g compound enzyme, and 400g phosphate buffer were treated on a shaker at 150rpm and 42℃ for 4 hours. The pH was adjusted to 7.0 with 0.1mol / L NaOH aqueous solution. The mixture was centrifuged at 4000rpm for 1 minute and dried at 40℃ for 10 hours to obtain enzymatically hydrolyzed starch. The compound enzyme was a mixture of α-amylase, β-amylase, and pullulanase in a mass ratio of 1:1:2.
[0104] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 35°C for 20 minutes to prepare a 10wt% mixture, and adjust the pH to 10 with 0.1mol / L NaOH aqueous solution; mix 2g of dodecenyl succinic anhydride with 4g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate at 400W for 8 minutes after each addition of treatment agent. After each sonication, adjust the pH to 10 again with 0.1mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 20 minutes, adjust the pH to 6.5 with 0.1mol / L hydrochloric acid, centrifuge at 4000rpm for 10 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 40°C for 12 hours, and pass through a 150-mesh sieve to obtain modified starch;
[0105] S3. Prepare a 5wt% mixture by adding modified starch to water; add 4g of chitosan to 300g of 2wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 1g of buffalo horn powder to 50g of water and stir evenly to obtain buffalo horn powder solution; mix the above three liquids, stir at 500rpm for 30 minutes, centrifuge at 4000rpm for 10 minutes, collect the precipitate, dry at 40℃ for 12 hours, and pass through a 150-mesh sieve to obtain the stabilizer.
[0106] Comparative Example 1
[0107] The preparation method of the longevity tonic juice is basically the same as that in Example 1, except that the preparation method of the stabilizer is different.
[0108] The stabilizer is prepared as follows:
[0109] S1. 40g wheat starch, 1.2g compound enzyme, and 400g phosphate buffer were treated on a shaker at 150rpm and 42℃ for 4 hours. The pH was adjusted to 7.0 with 0.1mol / L NaOH aqueous solution. The mixture was centrifuged at 4000rpm for 1 minute and dried at 40℃ for 10 hours to obtain enzymatically hydrolyzed starch. The compound enzyme was a mixture of α-amylase, β-amylase, and pullulanase in a mass ratio of 1:1:2.
[0110] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 35°C for 20 minutes to prepare a 10wt% mixture, and adjust the pH to 10 with 0.1mol / L NaOH aqueous solution; mix 2g of octenyl succinic anhydride with 4g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate at 400W for 8 minutes after each addition of treatment agent. After each sonication, adjust the pH to 10 again with 0.1mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 20 minutes, adjust the pH to 6.5 with 0.1mol / L hydrochloric acid, centrifuge at 4000rpm for 10 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 40°C for 12 hours, and pass through a 150-mesh sieve to obtain modified starch;
[0111] S3. Prepare a 5wt% mixture by adding modified starch to water; add 4g of chitosan to 300g of 2wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 1g of pearl powder to 50g of water and stir evenly to obtain a pearl powder solution; mix the above three liquids, stir at 500rpm for 30 minutes, centrifuge at 4000rpm for 10 minutes, collect the precipitate, dry at 40℃ for 12 hours, and pass through a 150-mesh sieve to obtain the stabilizer.
[0112] Comparative Example 2
[0113] The preparation method of the longevity tonic juice is basically the same as that in Example 1, except that the preparation method of the stabilizer is different.
[0114] The stabilizer is prepared as follows:
[0115] S1. 40g wheat starch, 1.2g compound enzyme, and 400g phosphate buffer were treated on a shaker at 150rpm and 42℃ for 4 hours. The pH was adjusted to 7.0 with 0.1mol / L NaOH aqueous solution. The mixture was centrifuged at 4000rpm for 1 minute and dried at 40℃ for 10 hours to obtain enzymatically hydrolyzed starch. The compound enzyme was a mixture of α-amylase, β-amylase, and pullulanase in a mass ratio of 1:1:2.
[0116] S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 35°C for 20 minutes to prepare a 10wt% mixture, and adjust the pH to 10 with 0.1mol / L NaOH aqueous solution; mix 2g of dodecenyl succinic anhydride with 4g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate at 400W for 8 minutes after each addition of treatment agent. After each sonication, adjust the pH to 10 again with 0.1mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 20 minutes, adjust the pH to 6.5 with 0.1mol / L hydrochloric acid, centrifuge at 4000rpm for 10 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 40°C for 12 hours, and pass through a 150-mesh sieve to obtain modified starch;
[0117] S3. Prepare a 5wt% mixture by adding modified starch to water; add 4g of chitosan to 300g of 2wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 1g of earthworm protein powder to 50g of water and stir evenly to obtain an earthworm protein powder solution; mix the above three liquids, stir at 500rpm for 30 minutes, centrifuge at 4000rpm for 10 minutes, collect the precipitate, dry at 40℃ for 12 hours, and pass through a 150-mesh sieve to obtain the stabilizer.
[0118] Comparative Example 3
[0119] The preparation method of the Longevity Tonic Juice is basically the same as that in Example 1, except that the stabilizer is not added.
[0120] Test Example 1
[0121] Stability test
[0122] I. Purpose of the Test
[0123] This stability test aims to evaluate the physicochemical stability and retention rate of active ingredients of the Longevity Tonic Juice under accelerated storage conditions, ensuring that the product maintains consistent quality, safety, and efficacy throughout its shelf life. The test simulates a high-temperature and high-humidity environment, monitoring changes in appearance, pH value, and the content of the key active ingredient (paeoniflorin), providing a scientific basis for setting the product's shelf life.
[0124] II. Test Conditions
[0125] Storage environment: A constant temperature and humidity chamber is used, with the temperature set at 40℃±2℃ and the relative humidity at 75%±5%RH.
[0126] Test duration: 6 months (180 days) of continuous storage, with periodic sampling and analysis.
[0127] Sample preparation: The test sample is the finished Shouxing supplement juice (specification: 1000mL / bottle) after filling, sealed and stored in a neutral glass container to avoid the influence of light.
[0128] III. Observation Indicators and Detection Methods
[0129] 1. Monitoring of Appearance Changes
[0130] Inspection items: color, transparency, sedimentation or layering.
[0131] Inspection methods: Visual observation and color comparison with standard color charts (such as Pantone color charts); transparency is quantified by a transmittance meter (wavelength 600nm); sedimentation is assessed by centrifugation (3000rpm, 10 minutes) followed by observation of the residue at the bottom.
[0132] 2. pH value change monitoring
[0133] Detection method: The pH value of the sample was directly measured using a calibrated precision pH meter (accuracy ±0.01). Triple parallel samples were measured each time, and the average value was taken.
[0134] 3. Content determination (quantitative determination of paeoniflorin)
[0135] Determination principle: Determined by high performance liquid chromatography (HPLC) according to General Chapter 0512 of the 2025 edition of the Chinese Pharmacopoeia.
[0136] Chromatographic conditions: Column: Octadecylsilane-bonded silica gel (C18 column, 250 mm × 4.6 mm, 5 μm). Mobile phase: Acetonitrile-0.1% phosphoric acid solution (14:86, v / v), isocratic elution. Flow rate: 1.0 mL / min. Detection wavelength: 230 nm. Column temperature: 30 °C. Injection volume: 10 μL.
[0137] Solution preparation: Reference solution: Take an appropriate amount of paeoniflorin reference standard (purity ≥98%), accurately weigh it, dissolve it in methanol and dilute it to prepare a solution containing 60 μg per 1 mL, and filter it through a 0.22 μm microporous membrane for later use.
[0138] Test solution: Accurately measure 10 mL of the Shouxing juice sample stored in a high temperature and high humidity environment, place it in a 50 mL volumetric flask, dilute with methanol to the mark, shake well, filter through a 0.22 μm microporous membrane, and take the filtrate as the test solution.
[0139] Determination method: Accurately pipette 10 μL each of the reference solution and the test solution into the liquid chromatograph, record the chromatogram, and calculate the paeoniflorin content by peak area according to the external standard method.
[0140] The test results are summarized in Table 1, including appearance, pH value, and paeoniflorin content.
[0141] Table 1
[0142]
[0143] Test Example 2
[0144] In vitro release rate determination:
[0145] The release behavior measurement procedure is as follows:
[0146] First, 10 mg of the Shouxing supplement sample from the embodiments and comparative examples of this invention was taken, and the absorbance of the supernatant was measured at 230 nm to obtain the concentration of paeoniflorin in the sample. 10 mL of 0.2 mol / L PBS buffer containing α-amylase (pH 7.2) was added, and the mixture was incubated at 37°C for 3 minutes by shaking, followed by centrifugation (5500 rpm, 10 minutes). The absorbance of the supernatant was measured at 230 nm to obtain the amount released in the oral cavity stage. The precipitate was resuspended in 10 mL of simulated gastric juice (3 g / L pepsin, 8.5 g / L NaCl, pH 1.6, adjusted with HCl), and incubated at 37°C for 60 minutes. The supernatant was centrifuged using the same method, and the absorbance at 230 nm was measured to calculate the gastric digestion release rate. Subsequently, the particles were treated with 10 mL of simulated intestinal juice (3 g / L bile salts, 10 g / L pancreatin, 0.2 mol / L PBS buffer, pH 7.5), digested at 37°C for 120 minutes, and the supernatant was measured using the same method to calculate the intestinal digestion release rate.
[0147] The relevant test data are summarized in Table 2.
[0148] Table 2
[0149]
[0150] The mechanism by which Example 1 exhibits better stability and in vitro release rate compared to Example 2 and Comparative Example 1 may be as follows: Dodecenyl succinic anhydride (C12 chain) has a moderately long hydrophobic chain, enabling efficient esterification with starch hydroxyl groups under alkaline conditions. This introduces carboxyl groups, making the starch negatively charged and forming a dense and stable interfacial film that effectively anchors the oil-water interface, preventing volatile oil escape and oxidation. In contrast, hexadecenyl succinic anhydride (C16 chain) suffers from incomplete esterification and particle aggregation due to its excessively long chain, while octenyl succinic anhydride (C8 chain) results in insufficient emulsification and a fragile interfacial film due to its excessively short chain. Simultaneously, the inorganic mineral properties (calcium carbonate) of mother-of-pearl powder provide a high specific surface area and porous structure. Through calcium ion bridging, it generates strong electrostatic interactions with the protonated amino groups of chitosan, forming a rigid complex that enhances the mechanical strength and pH buffering capacity of the interfacial film. This significantly reduces the content of peroxides and malondialdehyde under accelerated storage conditions, delays the degradation of paeoniflorin, and achieves a stable and sustained release. Compared with Examples 3, 4 and Comparative Example 2, the better effect of Example 1 may be due to the fact that the mineral matrix of pearl powder is superior to that of organic biological powders (polysaccharides from Gastrodia elata powder, proteins from buffalo horn powder and proteins from earthworm protein powder). Its calcium carbonate component lacks thermal denaturation and enzymatic hydrolysis sensitivity, and can maintain the integrity of the interface in gastric and intestinal juices, avoiding membrane damage caused by protein denaturation or polysaccharide hydrolysis, thereby providing better adsorption and stability, reducing the risk of burst release, improving bioavailability, and at the same time, the cost is low.
Claims
1. A method for preparing a longevity tonic, characterized in that, The method is as follows: The volatile oil and distillate of Angelica sinensis, cinnamon twig, and dried ginger are extracted by steam distillation and separated for later use. The residue is then decocted with yam, stir-fried hawthorn, prepared Polygonum multiflorum, Codonopsis pilosula, Poria cocos, stir-fried Atractylodes macrocephala, honey-processed licorice, stir-fried Paeonia lactiflora, Ophiopogon japonicus, and Rehmannia glutinosa. The decoction is filtered, concentrated, precipitated with alcohol, the ethanol is recovered, and then concentrated again. Sodium benzoate, stabilizer, polysorbate 80, the aforementioned volatile oil and distillate are added, stirred well, and brought to a final volume. The mixture is then bottled. The stabilizer is prepared by enzymatic hydrolysis of wheat starch with a compound enzyme, ultrasonic-assisted esterification modification with an acid anhydride compound, blending it with chitosan and biological powder, and then centrifuging, drying and sieving.
2. The method for preparing the longevity tonic juice as described in claim 1, characterized in that, The preparation method of the longevity tonic juice is as follows: This product is composed of 13 Chinese medicinal herbs, with the following specific ingredients and dosages: 200-280g of Chinese yam, 100-140g of stir-fried hawthorn, 100-140g of prepared Polygonum multiflorum, 180-220g of Codonopsis pilosula, 30-50g of Poria cocos, 20-30g of dried ginger, 70-90g of Angelica sinensis, 70-90g of cinnamon twig, 40-60g of stir-fried Atractylodes macrocephala, 40-60g of honey-processed licorice root, 40-60g of stir-fried white peony root, 40-60g of Ophiopogon japonicus, and 80-120g of prepared Rehmannia glutinosa. First, take Angelica sinensis, Cinnamomum cassia, and Zingiber officinale, and extract their volatile oil components using steam distillation. Separate the oil-water mixture produced during distillation, collecting the volatile oil and the distilled aqueous solution separately in dedicated containers. Add water to the remaining medicinal residue after volatile oil extraction and decoct twice with the other ten medicinal materials in the prescription. Combine the two decoctions, filter, and concentrate to 550-700 mL. Add 1.5-3 times the volume of anhydrous ethanol to the concentrate, stir to precipitate impurities, let stand, filter, recover the ethanol from the filtrate, dilute with 400-800g of water, filter again, and concentrate to 300-400 mL. Add 1-5g of sodium benzoate, along with the aforementioned distilled aqueous solution and its volatile oil, 1-5g of stabilizer, and 1-10g of polysorbate 80. Adjust the total volume to 1000 mL with water, stir well, and bottle to obtain the Longevity Tonic Juice.
3. The method for preparing the longevity tonic juice as described in claim 2, characterized in that, The first addition of water for decoction involves adding 10-15L of water and decocting for 2-6 hours.
4. The method for preparing the longevity tonic juice as described in claim 2, characterized in that, The second addition of water involves adding 5-10L of water and simmering for 1-5 hours.
5. The method for preparing the longevity tonic juice as described in claim 1 or 2, characterized in that, The stabilizer is prepared as follows: S1. Mix 20-50g wheat starch, 0.8-1.5g compound enzyme, and 300-500g phosphate buffer in a shaker at 100-300rpm and 40-45℃ for 2-6 hours. Adjust the pH to 6.5-7.5 with 0.05-0.2mol / L NaOH aqueous solution. Centrifuge at 3000-5000rpm for 0.5-3 minutes and dry at 30-45℃ for 5-12 hours to obtain enzymatically hydrolyzed starch. S2. Disperse the enzymatically hydrolyzed starch prepared in step S1 in water, stir at 30-40℃ for 10-30 minutes to prepare a 5-15wt% mixture, and adjust the pH to 9-10.5 with 0.05-0.2mol / L NaOH aqueous solution; mix 1-3g of acid anhydride compound with 2-6g of anhydrous ethanol, divide into three equal portions of treatment agent, and sonicate after each addition. After each sonication, adjust the pH to 9-10.5 again with 0.05-0.2mol / L NaOH aqueous solution. After all the treatment agent is added, stir magnetically for 10-30 minutes, adjust the pH to 6-6.8 with 0.05-0.2mol / L hydrochloric acid, centrifuge at 3000-5000rpm for 5-15 minutes, wash twice with water, then wash twice with anhydrous ethanol, dry at 30-45℃ for 5-20 hours, and pass through a 100-300 mesh sieve to obtain modified starch; S3. Prepare a 3-8 wt% mixture by adding modified starch to water; add 2-6 g of chitosan to 200-400 g of 1-3 wt% citric acid aqueous solution to prepare a chitosan aqueous solution; add 0.5-2 g of biological powder to 40-60 g of water and stir evenly to obtain a biological powder liquid; mix the above three liquids, stir at 300-800 rpm for 10-50 minutes, centrifuge at 3000-5000 rpm for 5-15 minutes, collect the precipitate, dry at 30-45℃ for 5-20 hours, and pass through a 100-300 mesh sieve to obtain the stabilizer.
6. The method for preparing the longevity tonic juice as described in claim 5, characterized in that, The complex enzyme is composed of α-amylase, β-amylase, and pullulanase mixed in a mass ratio of 0.5-2:0.5-2:1-3.
7. The method for preparing the longevity tonic juice as described in claim 5, characterized in that, In step S2, the ultrasonic treatment power is 200-600W and the time is 5-10 minutes.
8. The method for preparing the longevity tonic juice as described in claim 5, characterized in that, The anhydride compound is at least one of dodecenylsuccinic anhydride and hexadecenylsuccinic anhydride.
9. The method for preparing the longevity tonic juice as described in claim 5, characterized in that, The biological powder is at least one of buffalo horn powder, mother-of-pearl powder, and gastrodia elata powder.
10. A tonic juice for longevity, characterized in that, It is prepared by the preparation method described in any one of claims 1-9.