Fine extraction process of veterinary oral liquid for clearing pestilence and detoxifying

Abstract

The invention relates to the technical field of veterinary drugs, and provides a refined extraction process of veterinary oral liquid capable of clearing heat and detoxifying, which comprises the following steps: S1, mixing cape jasmine and fructus forsythiae, and extracting to obtain volatile oil; s2, mixing radix rehmanniae, radix isatidis, rhizoma corydalis and water, heating to boiling, adding radix scutellariae, performing reflux extraction, and filtering to obtain an extracting solution I and medicine residues; s3, mixing the medicine residues with water, performing reflux extraction, and filtering to obtain an extracting solution II; s4, mixing the extracting solution I and the extracting solution II, concentrating and filtering to obtain filtrate; s5, standing the filtrate, and collecting supernate; and S6, mixing the volatile oil with a surfactant, mixing with the supernatant, adjusting the pH value to 5-6, fixing the volume, and filtering to obtain the scourge-clearing and detoxification oral liquid. According to the technical scheme, the problems of low content of geniposide and baicalin and serious loss of volatile components of fructus gardeniae and fructus forsythiae in the scourge-clearing and detoxifying oral liquid in the prior art are solved.

Description

Technical Field

[0001] The invention relates to the technical field of veterinary drugs, and in particular to a refined extraction process of a veterinary Qingwen Jiedu oral liquid. Background Art

[0002] Qingwen Jiedu Oral Liquid is a prescription included in the second volume of the Chinese Veterinary Pharmacopoeia. It is a compound preparation composed of 6 herbs: Rehmannia glutinosa, Gardenia jasminoides, Scutellaria baicalensis, Forsythia suspensa, Scrophularia ningpoensis, and Radix Isatidis. It has the function of clearing away heat and detoxifying, and is mainly used to treat exogenous fever. It is commonly used clinically for Newcastle disease, influenza, larynx infection, bursal disease, and mixed infections caused by multiple pathogens, with symptoms such as fever, fatigue, cough, thirst, congestion and bleeding caused by excessive heat in the lungs and stomach, etc. In the formula, Gardenia is used heavily to clear the heat of the three burners, which can not only purge the heat evil of the heart and lungs, but also relieve the depressed fire of the three burners. It is good at clearing heat, purging fire and relieving restlessness, and it is the main medicine; Scutellaria baicalensis clears and purges lung heat, Forsythia suspensa clears the fire of the heart and lungs, disperses nodules and reduces swelling, Isatis root detoxifies and relieves sore throat, all of which are ministerial medicines, assisting the main medicine in clearing and resolving heat and toxicity in the middle and upper burners, Rehmannia root cools blood and nourishes yin, purges fire and relieves restlessness, Scrophularia ningpoensis strengthens kidney water to control heart fire, clears lung metal, and is good at purging rootless floating fire, all of which are adjuvant medicines, assisting the main medicine in reducing fire and relieving restlessness. All the medicines are used together to achieve the effect of purging fire and detoxifying.

[0003] Traditional Qingwen Jiedu oral liquid process: add water to the prescription amount of medicinal materials and boil them twice, combine the decoction, stand, filter, concentrate, filter again, add sodium benzoate, fix the volume, fill, sterilize, and obtain. The preparation process is only a water extraction and standing impurity removal process. Although the process is simple, the extraction rate of the active ingredients of Radix Isatidis and Radix Scutellariae in the product is low, the volatile components of Gardenia and Fructus Forsythiae are seriously lost, and the liquid has many impurities. Chinese patent CN102319354A discloses a Qingre Jiedu oral liquid and a preparation method thereof, which uses alcohol precipitation and two clarifiers for impurity removal. Although the clarification effect is very good, the preparation process is cumbersome, and the 101 juice clarifier added with the feed cannot play an effective clarification effect due to filtration, and the baicalin content is low due to continuous impurity removal, the cycle is long, the manufacturing cost is high, and it is not suitable for economic animals. Summary of the invention

[0004] The present invention proposes a refined extraction process for a Qingwen Jiedu oral liquid for animals, which solves the problems of low content of gardenia glycoside and baicalin and serious loss of volatile components of gardenia and forsythia in the Qingwen Jiedu oral liquid in the related art.

[0005] The technical solution of the present invention is as follows: A refined extraction process of a veterinary Qingwen Jiedu oral liquid comprises the following steps: S1. Mixing Gardenia jasminoides and Forsythia suspensa and extracting to obtain volatile oil; S2, mixing Rehmannia root, Radix Isatidis, and Radix Glehniae with water, heating to boiling, adding Scutellaria baicalensis for reflux extraction, filtering, and obtaining extract I and medicinal residues; S3, mixing the medicinal residue with water, performing reflux extraction, and filtering to obtain extract II; S4, after mixing the extract I and the extract II, concentrating and filtering to obtain a filtrate; S5, allowing the filtrate to stand and collecting the supernatant; S6. After mixing the volatile oil with the surfactant, mix it with the supernatant, adjust the pH to 5-6, fix the volume, filter, and obtain the Qingwen Jiedu oral liquid.

[0006] As a further technical solution, the fixed volume is 1000L of oral liquid for every 1175~1450kg of total medicinal materials.

[0007] As a further technical solution, the extraction in S1 is carried out in a special volatile oil collection equipment (including an oil-water rheometer, a condenser, an oil-water separator), etc., and the parameters are set to a steam flow rate of 100 kg / h. The timing starts from the appearance of reflux liquid in the reflux pipe. After 2 hours, the direct steam switch is closed to stop collecting volatile oil.

[0008] As a further technical solution, the reflux extraction in S2 and S3 is carried out in a dynamic hot reflux extraction tank.

[0009] As a further technical solution, the temperature of the water in S2 is 40-60°C.

[0010] The inventors found that when Isatis root was soaked in cold water, the active ingredient Epigoitrin in the Isatis root would be removed along with the impurities, so the water temperature was limited to 40~60℃, ensuring the effective extraction of Epigoitrin in the refining process of Qingwen Jiedu oral liquid.

[0011] As a further technical solution, before standing in S5, the filtrate is further mixed with a clarifier solution.

[0012] As a further technical solution, the clarifier solution is a clarifier aqueous solution, and the mass volume ratio of the clarifier to water in the clarifier aqueous solution is 1kg:3~8L. As a further technical solution, the clarifier can be any type of clarifier, preferably ZTC-101 juice clarifier.

[0013] As a further technical solution, before S6 is mixed with the supernatant, the supernatant is transferred to a centrifuge for centrifugation, and then the supernatant is collected again for filtration.

[0014] The present invention clarifies the medicinal liquid by combining a clarifier with a centrifuge, thereby minimizing the loss of effective ingredients, while clarifying the medicinal liquid, thereby increasing the content and stability of baicalin and gardenia jasminoides in the Qingwen Jiedu oral liquid.

[0015] As a further technical solution, the centrifuge is a butterfly centrifuge. Preferably, the parameters are set as: online cleaning 15 minutes, sealing time 10 seconds, slag discharge time 2.0 seconds, water replenishment time 5 seconds, feeding time 5 to 20 minutes, water replenishment time 3 minutes, vibration protection value 12.0 nn / s, and feeding frequency 50 Hz.

[0016] The present invention simplifies the clarification process by removing impurities with a butterfly centrifuge, and improves the content and stability of baicalin and gardenia jasminoides in the product.

[0017] As a further technical solution, the extraction in S1 is specifically: extraction by steam distillation, and the extraction time is 1 to 3 hours.

[0018] As a further technical solution, the mixture is soaked for 0.5 to 1.5 hours before heating in S2.

[0019] As a further technical solution, the mass ratio of Rehmannia root, Gardenia jasminoides, Scutellaria baicalensis, Fructus Forsythiae, Scrophularia ningpoensis and Radix Isatidis is 3~4:5~6:4.5~5:4~5:3~4:4~5.

[0020] As a further technical solution, the amount of water used in S2 and S3 is independently 6 to 9 times the total mass of Rehmannia root, Gardenia jasminoides, Scutellaria baicalensis, Forsythia suspensa, Scrophularia ningpoensis and Radix Isatidis.

[0021] As a further technical solution, the concentration in S4 is reduced-pressure concentration, and the temperature of the reduced-pressure concentration is 60-80° C. and the pressure is -0.06--0.08 MPa.

[0022] As a further technical solution, the volume ratio of the volatile oil to the surfactant is 1:0.5~1.5.

[0023] As a further technical solution, the surfactant can be any type of surfactant, preferably Tween 80.

[0024] The working principle and beneficial effects of the present invention are: 1. The present invention extracts volatile oil separately, accurately formulates the order of adding medicine, extraction method and impurity removal scheme, follows the "decoction first" and "add later" order of medicine preparation in the traditional Chinese medicine preparation process, and solves the problems of loss of effective ingredients of individual medicinal materials during extraction and mutual influence of various medicinal materials; the process of the present invention is simple, the production cycle is short, the production can be scaled up, and the operating cost is low. The Qingwen Jiedu oral liquid prepared by this method has high content of effective ingredients and good stability, which overcomes the shortcomings and deficiencies of the existing Qingwen Jiedu oral liquid preparation process.

[0025] 2. The refined extraction process of the veterinary Qingwen Jiedu oral liquid provided by the present invention avoids the problem that most of the volatile oil components in Gardenia and Forsythia suspensa are lost with water vapor according to the conventional water extraction method. It is very important to retain the effective ingredients of the volatile oil by collecting the volatile oil separately, and the volatile components in Gardenia and Forsythia suspensa are retained to the maximum extent.

[0026] 3. The present invention first adds Gardenia and Forsythia to collect volatile oil, then adds Rehmannia root, Isatis root, and Scrophularia ningpoensis for warm soaking, and after boiling, adds Scutellaria baicalensis in the order of adding medicine, so as to achieve the best extraction method of single medicinal materials and maximize the extraction rate of effective ingredients of medicinal materials, and adopts the dynamic reflux concentration extraction method of extracting and concentrating at the same time (completed by a dynamic hot reflux extraction concentration tank) to concentrate it, thereby achieving simultaneous extraction and concentration.

[0027] 4. In the extraction process, the present invention studies the optimal feeding sequence, extraction method, extraction temperature, extraction time, impurity removal scheme and other preparation parameter indicators according to the characteristics of the materials. The factors affecting the content of the effective ingredients in the Qingwen Jiedu oral liquid during the extraction process are the feeding sequence and extraction method. During the experiment, the inventors found that Scutellaria baicalensis contains decomposition enzymes, which are easily decomposed and oxidized into quinone derivatives in an aqueous solution at a temperature below 80°C, so the feeding sequence and temperature are crucial. DETAILED DESCRIPTION

[0028] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0029] The parameters of the disc centrifuge in the following embodiments and comparative examples are set as follows: online cleaning 15 minutes; sealing time 10 seconds; slag discharge time 2.0 seconds; water replenishment time 5 seconds; water replenishment time 3 minutes; and vibration protection value 12.0 nn / s.

[0030] Example 1 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis indigotica, 1kg ZTC-101 juice clarifier.

[0031] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to an oil-water rheometer and pass water vapor. The steam flow rate is controlled at 100 kg / h. The timing starts from the appearance of reflux liquid in the reflux pipe. After 2 hours, the direct steam switch is closed to separate the volatile oil from the oil-water separator and store in a sealed refrigerator. S2. Mix Scrophularia, Radix Isatidis, Radix Rehmanniae and 9400 kg of water in a dynamic hot reflux extraction tank, turn on the steam heating to boiling, add Scutellaria baicalensis, use the dynamic hot reflux extraction tank to extract for 1.5 hours, filter, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again and boil for 1.5 hours, filter, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 80° C. and -0.06 MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75 μm plate and frame filter to obtain a filtrate; S4, add 5L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S5, the supernatant is fed through a disc centrifuge at a frequency of 50 Hz for 15 minutes according to the set feeding time. After centrifugation, the supernatant is passed through a double-layer 200-mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S6. Mix the volatile oil with Tween 80 in a volume ratio of 1:1, stir evenly, add to the liquid preparation tank, adjust the pH to 5.5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0032] Example 2 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis root.

[0033] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to an oil-water rheometer and pass water vapor. The steam flow rate is controlled at 100 kg / h. The timing starts from the appearance of reflux liquid in the reflux pipe. After 2 hours, the direct steam switch is closed to separate the volatile oil from the oil-water separator and store in a sealed refrigerator. S2. After heating 9400 kg of water to 50° C., mix it with Scrophularia ningpoensis, Radix Isatidis, and Rehmannia glutinosa in a dynamic hot reflux extraction tank. After warm soaking for 1 hour, turn on the steam heating to boiling and add Scutellaria baicalensis. Use the dynamic hot reflux extraction tank to extract for 1.5 hours, filter, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again and boil it for 1.5 hours, filter, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 80°C and -0.06MPa to obtain a concentrate, and after the concentrate is cooled, filtering it with a 75μm plate and frame filter to obtain a filtrate, letting it stand for 12h, and taking the supernatant; S4, the supernatant is filtered through a double layer of 200 mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S5. Mix the volatile oil with Tween 80 in a volume ratio of 1:1, stir evenly, add to the liquid preparation tank, adjust the pH to 5.5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0034] Example 3 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis indigotica, 1kg ZTC-101 juice clarifier.

[0035] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to an oil-water rheometer and pass water vapor. The steam flow rate is controlled at 100 kg / h. The timing starts from the appearance of reflux liquid in the reflux pipe. After 2 hours, the direct steam switch is closed to separate the volatile oil from the oil-water separator and store in a sealed refrigerator. S2. After heating 9400 kg of water to 50° C., mix it with Scrophularia ningpoensis, Radix Isatidis, and Rehmannia glutinosa in a dynamic hot reflux extraction tank. After warm soaking for 1 hour, turn on the steam heating to boiling and add Scutellaria baicalensis. Use the dynamic hot reflux extraction tank to extract for 1.5 hours, filter, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again and boil it for 1.5 hours, filter, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 80° C. and -0.06 MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75 μm plate and frame filter to obtain a filtrate; S4, add 5L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S5, the supernatant is filtered through a double-layer 200-mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S6. Mix the volatile oil with Tween 80 in a volume ratio of 1:1, stir evenly, add to the liquid preparation tank, adjust the pH to 5.5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0036] Example 4 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis indigotica, 1kg ZTC-101 juice clarifier.

[0037] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to an oil-water rheometer and pass water vapor. The steam flow rate is controlled at 100 kg / h. The timing starts from the appearance of reflux liquid in the reflux pipe. After 2 hours, the direct steam switch is closed to separate the volatile oil from the oil-water separator and store in a sealed refrigerator. S2. After heating 9400 kg of water to 50° C., mix it with Scrophularia ningpoensis, Radix Isatidis, and Rehmannia glutinosa in a dynamic hot reflux extraction tank. After warm soaking for 1 hour, turn on the steam heating to boiling and add Scutellaria baicalensis. Use the dynamic hot reflux extraction tank to extract for 1.5 hours, filter, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again and boil it for 1.5 hours, filter, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 80° C. and -0.06 MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75 μm plate and frame filter to obtain a filtrate; S4, add 5L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S5, the supernatant is fed through a disc centrifuge at a frequency of 50 Hz according to the set feeding time of 5-20 minutes. After centrifugation, the supernatant is passed through a double-layer 200-mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S6. Mix the volatile oil with Tween 80 in a volume ratio of 1:1, stir evenly, add to the liquid preparation tank, adjust the pH to 5.5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0038] Example 5 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis indigotica, 1kg ZTC-101 juice clarifier.

[0039] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to the oil-water rheometer and pass water vapor, the steam flow rate is controlled at 100 kg / h, start timing from the appearance of reflux liquid in the reflux pipe, close the direct steam switch after 1 hour, separate the volatile oil from the oil-water separator, and store in a sealed refrigerator; S2. After heating 7050 kg of water to 40°C, mix it with Scrophularia, Radix Isatidis, and Rehmannia in a dynamic hot reflux extraction tank, soak it for 0.5 h, turn on the steam heating until it boils, add Scutellaria baicalensis, use the dynamic hot reflux extraction tank to extract for 1.5 h, filter, and obtain extract I and filter residue; add 5400 kg of water to the filter residue and boil it for 1.5 h, filter, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 60° C. and -0.06 MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75 μm plate and frame filter to obtain a filtrate; S4, add 3L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S5, the supernatant is fed through a disc centrifuge at a frequency of 50 Hz according to the set feeding time of 5-20 minutes. After centrifugation, the supernatant is passed through a double-layer 200-mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S6. Mix the volatile oil with Tween 80 at a volume ratio of 1:0.5 and stir evenly, then add it to the liquid preparation tank, adjust the pH to 5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0040] Example 6 Raw materials: 200kg Rehmannia root, 300kg Gardenia jasminoides, 250kg Scutellaria baicalensis, 250kg Forsythia suspensa, 200kg Scrophularia ningpoensis, 250kg Isatis root, 1kg ZTC-101 juice clarifier.

[0041] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to an oil-water rheometer and pass water vapor, the steam flow rate is controlled at 100 kg / h, start timing from the appearance of reflux liquid in the reflux pipe, close the direct steam switch after 3 hours, separate the volatile oil from the oil-water separator, and store in a sealed refrigerator; S2. After heating 13050 kg of water to 60° C., mix it with Scrophularia ningpoensis, Radix Isatidis, and Radix Rehmanniae in a dynamic hot reflux extraction tank, soak it for 1.5 hours, turn on the steam heating until it boils, add Scutellaria baicalensis, extract it for 1.5 hours in a dynamic hot reflux extraction tank, filter it, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again, boil it for 1.5 hours, filter it, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 70°C and -0.08MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75μm plate and frame filter to obtain a filtrate; S4, add 8L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S5, the supernatant is fed through a disc centrifuge at a frequency of 50 Hz according to the set feeding time of 5-20 minutes. After centrifugation, the supernatant is passed through a double-layer 200-mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S6. Mix the volatile oil with Tween 80 at a volume ratio of 1:1.5 and stir evenly, then add it to the liquid preparation tank, adjust the pH to 5.5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0042] Comparative Example 1 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis root.

[0043] Process: S1. Add Rehmannia root, Gardenia jasminoides, Scutellaria baicalensis, Fructus Forsythiae, Scrophularia ningpoensis, Radix Isatidis and 9400 kg of water into a dynamic hot reflux extraction tank, extract for 1.5 h using the dynamic hot reflux extraction tank, filter to obtain extract I and filter residue; add 9400 kg of water to the filter residue again, boil for 1.5 h, filter to obtain extract II; S2. Add extract I and extract II into a concentration tank, and concentrate under reduced pressure at 80°C and -0.06MPa to obtain a concentrate. After the concentrate is cooled, filter it using a 75μm plate and frame filter to obtain a filtrate. After adjusting the pH to 5.5, the volume is fixed to 1000L to obtain the Qingwen Jiedu oral solution.

[0044] Comparative Example 2 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis indigotica, 1kg ZTC-101 juice clarifier.

[0045] Process: S1. After heating 9400 kg of water to 50°C, mix it with Scrophularia, Radix Isatidis, Rehmannia, Gardenia, and Fructus Forsythiae in a dynamic hot reflux extraction tank. After warm soaking for 1 hour, turn on the steam heating to boiling and add Scutellaria baicalensis. Use the dynamic hot reflux extraction tank to extract for 1.5 hours, filter, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again and boil for 1.5 hours, filter, and obtain extract II; S2, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 80° C. and -0.06 MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75 μm plate and frame filter to obtain a filtrate; S3, add 5L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S4. Feed the supernatant through a disc centrifuge at a frequency of 50 Hz for a set feeding time of 5-20 minutes. After centrifugation, take the supernatant and pass it through a double-layer 200-mesh filter cloth into a liquid preparation tank. Discard the bottom precipitate. Adjust the pH in the liquid preparation tank to 5.5, fix the volume to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0046] Comparative Example 3 Raw materials: 150kg Rehmannia root, 250kg Gardenia jasminoides, 225kg Scutellaria baicalensis, 200kg Forsythia suspensa, 150kg Scrophularia ningpoensis, 200kg Isatis indigotica, 1kg ZTC-101 juice clarifier.

[0047] Process: S1. Crush Gardenia jasminoides and Forsythia suspensa to less than 10 mesh, transfer to an oil-water rheometer and pass water vapor. The steam flow rate is controlled at 100 kg / h. The timing starts from the appearance of reflux liquid in the reflux pipe. After 2 hours, the direct steam switch is closed to separate the volatile oil from the oil-water separator and store in a sealed refrigerator. S2. After heating 9400 kg of water to 50° C., mix it with Scrophularia, Radix Isatidis, Radix Rehmanniae, and Radix Scutellariae in a dynamic hot reflux extraction tank. After warm soaking for 1 hour, turn on the steam to heat to boiling, extract it in a dynamic hot reflux extraction tank for 1.5 hours, filter, and obtain extract I and filter residue; add 9400 kg of water to the filter residue again, boil it for 1.5 hours, filter, and obtain extract II; S3, adding extract I and extract II into a concentration tank, and concentrating under reduced pressure at 80° C. and -0.06 MPa to obtain a concentrated solution, and after the concentrated solution is cooled, filtering it with a 75 μm plate and frame filter to obtain a filtrate; S4, add 5L of water to ZTC-101 juice clarifier, stir to adjust to paste, add to the filtrate, start stirring for 15min, stop stirring, let stand for 12h, and take the supernatant; S5, the supernatant is fed through a disc centrifuge at a frequency of 50 Hz according to the set feeding time of 5-20 minutes. After centrifugation, the supernatant is passed through a double-layer 200-mesh filter cloth and poured into a liquid preparation tank, and the bottom sediment is discarded; S6. Mix the volatile oil with Tween 80 in a volume ratio of 1:1, stir evenly, add to the liquid preparation tank, adjust the pH to 5.5, make the volume up to 1000 L, filter with a double-layer 200-mesh filter cloth, fill and sterilize to obtain the Qingwen Jiedu oral liquid.

[0048] The properties of the Qingwen Jiedu oral liquid obtained in Examples 1 to 6 and Comparative Examples 1 to 3 were measured for 6 months to evaluate stability. At the same time, the content of baicalin and gardenia jasminoides was measured by liquid phase method, the content of 4-methylisophorone and α-pinene and β-pinene was measured by gas phase method, and the content of epigoitrin was measured by thin layer chromatography. The results are recorded in Table 1.

[0049] Table 1 Statistical table of stability investigation data of Qingwen Jiedu oral liquid

[0050] As can be seen from Table 1, the collection amounts of 4-methenylisophorone of the Gardenia volatile oil and α-pinene and β-pinene of the Forsythia suspensa volatile oil in the Qingwen Jiedu oral liquid obtained in Examples 1 to 6 of the present invention are relatively high; and the contents of the effective ingredients baicalin and gardenia glycoside are relatively high, with the content of baicalin being above 9.3 mg / mL and the content of gardenia glycoside being above 5.5 mg / mL.

[0051] Comparative Example 1 adopts the traditional extraction process, and the contents of the effective ingredients baicalin and gardenia jasminoides are significantly low. The main reason is that the present invention follows the traditional Chinese medicine preparation method of "first decocting, then adding" according to the drug characteristics, and does not remove impurities.

[0052] Compared with Comparative Example 2, in Example 4, volatile oils were collected separately, and the obtained Qingwen Jiedu oral liquid contained 4-methylisophorone of Gardenia volatile oil, and α-pinene and β-pinene of Forsythia suspensa volatile oil, indicating that collecting volatile oils separately can avoid the loss of volatile oil components in Gardenia jasminoides and Forsythia suspensa medicinal materials.

[0053] Compared with Comparative Example 3, in Example 4, Rehmannia root, Isatis root and Scrophularia ningpoensis are added first and Scutellaria baicalensis is added last. The contents of baicalin and gardenia jasminoides in the obtained Qingwen Jiedu oral liquid are higher than those in Comparative Example 3, and it is still clear after 6 months, indicating that adding Rehmannia root, Isatis root and Scrophularia ningpoensis first and then adding Scutellaria baicalensis can improve the content and stability of baicalin and gardenia jasminoides in the Qingwen Jiedu oral liquid.

[0054] Compared with Example 1, in Example 4, water is first heated to 50°C and then mixed with Scrophularia ningpoensis, Isatis root and Rehmannia glutinosa in a tank. The obtained Qingwen Jiedu oral liquid contains epigoitrin, which indicates that heating the water to 50°C first can optimally extract epigoitrin, the medicinal ingredient in Isatis root.

[0055] Compared with Example 2, in Example 4, ZTC-101 juice clarifier was added and a disc centrifuge was used. The contents of baicalin and gardenoside in the obtained Qingwen Jiedu oral liquid were higher than those in Example 2, and it was still clear after 6 months, indicating that the combined use of the clarifier and the disc centrifuge can improve the content and stability of baicalin and gardenoside in the Qingwen Jiedu oral liquid.

[0056] Compared with Example 3, the content of baicalin and gardenia jasminoides in the Qingwen Jiedu oral liquid obtained by using a disc centrifuge in Example 4 is higher than that in Example 3, and it is still clear after 6 months, indicating that the use of a disc centrifuge can improve the content and stability of baicalin and gardenia jasminoides in the Qingwen Jiedu oral liquid.

[0057] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A refined extraction process for veterinary Qingwen Jiedu oral liquid, characterized in that: The following steps are involved: S1. Mixing Gardenia jasminoides and Forsythia suspensa and extracting to obtain volatile oil; S2, mixing Rehmannia root, Radix Isatidis, and Radix Glehniae with water, heating to boiling, adding Scutellaria baicalensis for reflux extraction, filtering, and obtaining extract I and medicinal residues; S3, mixing the medicinal residue with water, performing reflux extraction, and filtering to obtain extract II; S4, after mixing the extract I and the extract II, concentrating and filtering to obtain a filtrate; S5, allowing the filtrate to stand and collecting the supernatant; S6. After mixing the volatile oil with the surfactant, mix it with the supernatant, adjust the pH to 5-6, fix the volume, filter, and obtain the Qingwen Jiedu oral liquid.

2. The refined extraction process of the Qingwenjiedu oral liquid for animals according to claim 1, characterized in that: The temperature of the water in S2 is 40-60°C.

3. The refined extraction process of the Qingwen Jiedu oral liquid for animals according to claim 2, characterized in that: Before standing in S5, the filtrate is mixed with a clarifier solution.

4. The refined extraction process of the Qingwen Jiedu oral liquid for animals according to claim 3, characterized in that: Before S6 is mixed with the supernatant, the supernatant is transferred to a centrifuge for centrifugation, and then the supernatant is collected again for filtration.

5. The refined extraction process of the Qingwen Jiedu oral liquid for animals according to claim 1, characterized in that: The extraction in S1 is specifically: extraction by steam distillation, and the extraction time is 1 to 3 hours.

6. The refined extraction process of the Qingwenjiedu oral liquid for animals according to claim 2, characterized in that: Soak for 0.5 to 1.5 hours before heating in S2.

7. The refined extraction process of the Qingwenjiedu oral liquid for animals according to claim 1, characterized in that: The mass ratio of the rehmannia root, gardenia jasmine, scutellaria baicalensis, forsythia suspensa, figwort and isatis root is 3-4:5-6:4.5-5:4-5:3-4:4-5.

8. The refined extraction process of the Qingwenjiedu oral liquid for animals according to claim 1, characterized in that: The amount of water used in S2 and S3 is independently 6 to 9 times the total mass of Rehmannia root, Gardenia jasminoides, Scutellaria baicalensis, Forsythia suspensa, Scrophularia ningpoensis and Radix Isatidis.

9. The refined extraction process of the Qingwenjiedu oral liquid for animals according to claim 1, characterized in that: The concentration in S4 is reduced pressure concentration, and the temperature of the reduced pressure concentration is 60-80° C. and the pressure is -0.06--0.08 MPa.

10. The refined extraction process of the Qingwenjiedu oral liquid for animals according to claim 1, characterized in that: The volume ratio of the volatile oil to the surfactant is 1:0.5-1.5.

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