CN105535146B - Pretreatment method of radix puerariae, radix scutellariae and rhizoma coptidis composition medicinal materials - Google Patents
Pretreatment method of radix puerariae, radix scutellariae and rhizoma coptidis composition medicinal materials Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/488—Pueraria (kudzu)
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- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
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- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/539—Scutellaria (skullcap)
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- A61K36/71—Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
- A61K36/718—Coptis (goldthread)
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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Abstract
The invention relates to a pretreatment method of a medicinal material with a Gegen Qinlian formula, which comprises four working procedures of chopping, spraying and humidifying, extruding and puffing and fumigating. The principle is that the plant fiber of the medicinal material is destroyed through an extrusion and expansion process, so that the effective part of the medicinal material is contacted with the extracting solution in the subsequent extraction process in a larger area; part of organic matters in the medicinal materials are activated through the fumigation process, even reach a free state, and when the medicinal materials are extracted, effective components are easily separated from the medicinal materials and enter an extracting solution. Compared with the traditional method, the method has the advantage that the active ingredients of the medicine materials pretreated by the method can obtain higher extraction rate under the same extraction process and conditions.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a pretreatment method of a radix puerariae, radix scutellariae and rhizoma coptidis formula medicinal material.
Background
The pueraria root, scutellaria and coptis decoction is a famous prescription in Chinese traditional medicine, and is prepared by decocting 24g of pueraria root, 9g of huangfen, 9g of coptis root and 6g of liquorice with water. According to the records of the taiyang syndrome and pulse treatment of typhoid fever: taiyang disease, Gui Zhi syndrome, contrarily descending and then treating with diuresis. The rapid pulse, the exterior is not yet understood; it is indicated for dyspnea with sweating and is indicated for jin Ge Gen Qin Lian Tang. "
In order to adapt to the development of modern traditional Chinese medicine and bring convenience to people to take, pharmaceutical researchers develop dosage forms such as oral liquid, granules, capsules, pills, tablets, powder and the like according to the famous prescription of the traditional Chinese medicine, namely the 'Gegen Qinlian decoction'.
Regarding the Gegenqinlian Wan, its prescription and preparation method are described on page 1581 of the Chinese pharmacopoeia 2015 edition. Wherein, the extraction process of the active ingredients comprises the following steps: 1000g of kudzuvine root, 375g of baical skullcap root, 375g of golden thread and 250g of honey-fried licorice root; soaking Scutellariae radix and Coptidis rhizoma in 50% ethanol for 24 hr, percolating, collecting percolate, recovering ethanol, and concentrating; decocting radix Puerariae in water for 30min, adding Scutellariae radix, Coptidis rhizoma residue and radix Glycyrrhizae Preparata, decocting for 1.5 hr twice, mixing decoctions, filtering, concentrating the filtrate to appropriate amount, adding the above concentrated solution, and concentrating to obtain soft extract.
Chinese patent document CN101156906B discloses an extraction process of a radix puerariae and radix scutellariae medicine composition, which specifically comprises the following steps: (1) decocting radix Puerariae, Scutellariae radix, and Coptidis rhizoma with water, refluxing with ethanol, ultrasonic extracting or percolating to obtain radix Puerariae crude extract, Scutellariae radix crude extract and Coptidis rhizoma crude extract, respectively, and extracting Glycyrrhrizae radix with dilute ammonia water as solvent by refluxing or ultrasonic extracting to obtain Glycyrrhrizae radix crude extract; (2) refining the kudzu root crude extract obtained in the step (1) by using a macroporous resin method or an extraction method, refining the scutellaria baicalensis crude extract by using an acid precipitation method or a macroporous resin method, refining the coptis chinensis crude extract by using an acid precipitation method or a salting-out method, and refining the liquorice crude extract by using an acid precipitation method or a macroporous resin method.
Chinese patent document CN101156907B discloses a preparation method of a pueraria root scutellaria and coptis medicinal extract, which specifically comprises the following steps: (1) mixing the raw materials according to the weight ratio of kudzu root, scutellaria baicalensis, coptis chinensis and liquorice of 8: 3: 2, adding 6-12 times of water for decocting for 0.5-1.5 h, filtering, adding 4-10 times of water into filter residues for decocting for 0.5-1.5 h, filtering, combining the two filtrates, concentrating to 1/4-1/3 of the original volume, adding concentrated hydrochloric acid to adjust the pH to 1-2, standing for 12-24 h, and separating precipitates and supernate; washing the precipitate with water to a pH value of 5-6 for later use; adjusting the pH of the supernatant to 5-6, concentrating to a density of 1.10-1.20, adding ethanol until the ethanol content is 65-75%, filtering, and concentrating the filtrate to 1/3-1/2 of the weight of the medicinal materials to obtain a concentrated solution for later use. (2) Taking the concentrated solution to pass through a macroporous resin column, wherein the dosage of the resin is 1.3-3.0 times of the dosage of the medicinal materials; eluting with deionized water with the volume of 4-6 times of that of the column, eluting with 40% -70% ethanol with the volume of 3-5 times of that of the resin, collecting ethanol eluent, recovering the solvent under reduced pressure, mixing the extract with the precipitate obtained in the step (1), and drying to obtain the compound.
Therefore, in the published documents, the effective ingredients of the four medicinal materials of the root of kudzu vine, the root of baical skullcap, the rhizome of Chinese goldthread and the root of liquoric root are not processed before being extracted. The medicinal materials are generally dry medicinal materials in the medicinal material market. The inventor finds that in the actual production of the Gegenqinlian pill, a considerable part of active ingredients in the raw medicinal materials are still remained in the medicinal materials and are not extracted according to the operation of the method recorded in the Chinese pharmacopoeia 2015 edition, which causes great waste of traditional Chinese medicine resources.
Disclosure of Invention
The invention provides a pretreatment method of a medicinal material with a Gegenqinlian formula, aiming at improving the extraction rate of active ingredients of the medicinal material.
The invention relates to a pretreatment method of a medicinal material with a Gegen Qinlian formula, which comprises four working procedures of chopping, spraying and humidifying, extruding and puffing and fumigating. The four medicinal materials of the kudzuvine root, the baical skullcap root, the golden thread and the liquoric root can be mixed or respectively subjected to humidification, extrusion puffing and fumigation treatment.
The invention relates to a pretreatment method of a medicinal material with a Gegenqinlian formula, which comprises the following steps:
(1) weighing four medicinal materials of the root of kudzu vine, the root of large-flowered skullcap, the rhizome of Chinese goldthread and the root of liquoric root according to the weight ratio of 8: 3: 2, and cutting the medicinal materials into pieces of 3-5 cm;
(2) spraying and humidifying the cut medicinal materials in the step 1 until the water content of the medicinal materials is 8-16%;
(3) and (3) feeding the humidified medicine material obtained in the step (2) into a double-screw extrusion-expansion machine for extrusion expansion, wherein the expansion temperature is 35-60 ℃, and standing for 30-60 min.
(4) Sending the puffed medicinal materials into a closed container, fumigating for 5-30 min with saturated steam, and then performing an active ingredient extraction process.
Preferably, the pretreatment method of the radix puerariae, radix scutellariae and rhizoma coptidis composition medicinal materials comprises the following steps:
(1) weighing the medicinal materials of the root of kudzu vine, the scutellaria baicalensis, the coptis chinensis and the liquorice according to the weight ratio of 8: 3: 2, and cutting the medicinal materials into pieces of 3-5 cm;
(2) spraying and humidifying the cut medicinal materials in the step 1 until the water content of the medicinal materials is 8-14%;
(3) and (3) feeding the humidified medicine material obtained in the step (2) into a double-screw extrusion-expansion machine for extrusion expansion, wherein the expansion temperature is 45-60 ℃, and standing for 30-45 min.
(4) Sending the puffed medicinal materials into a closed container, fumigating the medicinal materials for 10 to 25min by saturated steam, and then entering an active ingredient extraction process.
Preferably, the pretreatment method of the radix puerariae, radix scutellariae and rhizoma coptidis composition medicinal materials comprises the following steps:
(1) weighing four medicinal materials of the root of kudzu vine, the root of large-flowered skullcap, the rhizome of Chinese goldthread and the root of liquoric root according to the weight ratio of 8: 3: 2, and cutting the medicinal materials into pieces of 3-5 cm;
(2) spraying and humidifying the cut medicinal materials in the step 1 until the water content of the medicinal materials is 12%;
(3) and (3) feeding the humidified medicine material obtained in the step (2) into a double-screw extrusion-expansion machine for extrusion expansion, wherein the expansion temperature is 55 ℃, and standing for 40 min.
(4) Sending the puffed medicinal materials into a closed container, fumigating with saturated steam for 15min, and extracting active ingredients.
The principle of the invention is that the plant fiber of the medicinal material is destroyed through the extrusion and expansion process, so that the effective part of the medicinal material is contacted with the extracting solution in the subsequent extracting process in a larger area; part of organic matters in the medicinal materials are activated through the fumigation process, even reach a free state, and when the medicinal materials are extracted, active ingredients are easily separated from the medicinal materials and enter an extracting solution. Compared with the traditional method, the active ingredients of the medicine materials pretreated by the method can obtain higher extraction rate under the same extraction process and conditions.
Detailed Description
Example 1
The pretreatment method of the medicinal materials with the Gegen Qinlian composition comprises the following steps:
(1) weighing four medicinal materials of the root of kudzu vine, the root of large-flowered skullcap, the rhizome of Chinese goldthread and the root of liquoric root according to the weight ratio of 8: 3: 2, and cutting the medicinal materials into pieces of 3-5 cm;
(2) spraying and humidifying the cut medicinal materials in the step 1 until the water content of the medicinal materials is 12%;
(3) and (3) feeding the humidified medicine material obtained in the step (2) into a double-screw extrusion-expansion machine for extrusion expansion, wherein the expansion temperature is 55 ℃, and standing for 40 min.
(4) Sending the puffed medicinal materials into a closed container, fumigating with saturated steam for 15min, and extracting active ingredients.
Examples 2 to 6
In examples 2 to 6, four process parameters of the water content, the expansion temperature, the standing time and the steam fumigation of the sprayed and humidified medicinal material are adjusted, and other operations are performed according to example 1.
The process parameters of each example are as follows:
the detection method comprises the following steps:
2kg of the Gegenqinlian formula medicine pretreated in the embodiment 1-6 is weighed, and the active ingredient fluid extract dry powder is prepared according to the extraction method of the Gegenqinlian active ingredient recorded in the Chinese pharmacopoeia 2015 edition.
The non-pretreated radix puerariae, radix scutellariae and rhizoma coptidis composition medicinal materials are prepared into active ingredient fluid extract dry powder serving as a reference sample according to an extraction method of active ingredients of radix puerariae, radix scutellariae and rhizoma coptidis recorded in Chinese pharmacopoeia 2015 edition.
Taking the dry extract powder of the examples and the reference samples, and measuring the content of each component according to the following method:
1. puerarin and its preparation method
Preparation of control solutions: taking a proper amount of puerarin reference substance, precisely weighing, and adding ethanol to prepare a solution containing 10 μ g of puerarin per 1 ml.
Preparation of test sample solution: precisely weighing 0.05g of dry powder of fluid extract in examples and reference samples, placing in a 100ml volumetric flask, adding appropriate amount of ethanol, performing ultrasonic treatment for 30min, standing at room temperature, adding ethanol to dilute to 100ml, shaking up, precisely sucking 1ml, and adding ethanol to dilute to 25 ml.
The determination method comprises the following steps: measuring the absorbances of the reference solution and the test sample solution at 250nm by using an ultraviolet spectrophotometry with ethanol as a blank, and calculating the content of the radix Puerariae total isoflavone according to the absorbances.
2. Baicalin
Preparation of control solutions: taking appropriate amount of baicalin control, precisely weighing, and adding ethanol to obtain solution containing 10 μ g of baicalin per 1 ml.
Preparation of test sample solution: accurately weighing 0.02g of dry powder of fluid extract of examples and reference samples into a 100ml volumetric flask, adding an appropriate amount of ethanol, carrying out water bath at 70 ℃ for 10min, carrying out ultrasonic treatment for 30min, standing to room temperature, adding ethanol to dilute to 100ml, shaking up, filtering, accurately sucking 5ml to 50ml of subsequent filtrate into the volumetric flask, adding ethanol to the scale, and shaking up.
The determination method comprises the following steps: measuring the absorbance of the reference solution and the test sample solution at 280nm by using an ultraviolet spectrophotometry with ethanol as a blank, and calculating the content of the total flavonoids in the scutellaria baicalensis according to the absorbance.
3. Berberine hydrochloride
Preparation of control solutions: taking a proper amount of berberine hydrochloride reference substance, precisely weighing, and adding ethanol to prepare a solution containing 10 μ g of berberine hydrochloride per 1 ml.
Preparation of test sample solution: precisely weighing 0.01g of dry powder of fluid extract of the examples and the reference sample, placing the dry powder in a 100ml volumetric flask, adding a proper amount of ethanol, carrying out water bath at 70 ℃ for 10min, carrying out ultrasonic treatment for 30min, placing the flask to room temperature, adding ethanol to dilute the solution to 100ml, shaking up the solution, precisely sucking 1ml of the solution, and adding ethanol to dilute the solution to 25 ml.
The determination method comprises the following steps: measuring absorbance of the reference solution and the test sample solution at 350nm by ultraviolet spectrophotometry with ethanol as blank, and calculating Coptidis rhizoma total alkaloid content according to absorbance.
4. Glycyrrhizic acid
Chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; methanol, 0.02mol/L ammonium acetate and glacial acetic acid (66: 33: 1) are taken as mobile phases; the detection wavelength is 254 nm; the theoretical plate number is not less than 3000 calculated according to ammonium glycyrrhizinate peak.
Preparation of control solutions: taking a proper amount of ammonium glycyrrhizinate reference substance, precisely weighing, and adding methanol to obtain a solution containing 50 μ g ammonium glycyrrhizinate per 1 ml.
Preparation of test sample solution: precisely weighing 0.02g of dry powder of fluid extract of the embodiment and the reference sample, placing the dry powder in a 100ml volumetric flask, adding a proper amount of methanol, carrying out water bath at 70 ℃ for 10min, carrying out ultrasonic treatment for 30min, placing the mixture to room temperature, adding methanol to dilute the mixture to a scale, shaking up, filtering, taking 1ml to 10ml of subsequent filtrate in the volumetric flask, and adding methanol to fix the volume.
The determination method comprises the following steps: precisely measuring 10 μ l of each of the reference solution and the test sample solution, injecting into a liquid chromatograph, measuring, and calculating glycyrrhizic acid content.
And (3) detection results:
and (3) comparing the results: (1) the extraction rate of the active ingredients of the Gegenqinlian drugs pretreated in the embodiments 1, 2, 3 and 6 of the invention is obviously improved compared with that of a reference sample; (2) the extraction rate of the active ingredients of the radix puerariae and radix scutellariae which are pretreated in the embodiments 3 and 6 is slightly improved compared with that of a reference sample; (3) the influence of the fumigation time on the extraction rate of the active ingredients is large, the activation effect of the active ingredients is not obvious if the fumigation time is short, and part of the active ingredients are leached out and lost by the condensed water during fumigation if the fumigation time is too long.
Claims (1)
1. A pretreatment method of a kudzu root, scutellaria baicalensis, coptis chinensis and liquorice prescription medicinal material is characterized by comprising the following steps of (1) weighing the kudzu root, the scutellaria baicalensis, the coptis chinensis and the liquorice respectively according to the weight ratio of 8: 3: 2, and cutting the kudzu root, the scutellaria baicalensis, the coptis chinensis and the liquorice into pieces of 3-5 cm; (2) spraying and humidifying the cut medicinal materials in the step 1 until the water content of the medicinal materials is 12%; (3) feeding the humidified medicinal materials in the step (2) into a double-screw extrusion puffing machine for extrusion puffing, wherein the puffing temperature is 55 ℃, and standing for 40 min; (4) sending the puffed medicinal materials into a closed container, fumigating with saturated steam for 15min, and extracting active ingredients.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101156907A (en) * | 2007-10-12 | 2008-04-09 | 南方医科大学 | A pueraria root scutellaria and coptis extract |
| CN104491041A (en) * | 2014-12-25 | 2015-04-08 | 江西心正药业有限责任公司 | Radix puerariae, astragalus membranaceus and coptis chinensis oral solution and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101156907A (en) * | 2007-10-12 | 2008-04-09 | 南方医科大学 | A pueraria root scutellaria and coptis extract |
| CN104491041A (en) * | 2014-12-25 | 2015-04-08 | 江西心正药业有限责任公司 | Radix puerariae, astragalus membranaceus and coptis chinensis oral solution and preparation method thereof |
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