CN111714465B - Jiuwei Shuangjie soft capsule and preparation method thereof - Google Patents

Jiuwei Shuangjie soft capsule and preparation method thereof Download PDF

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CN111714465B
CN111714465B CN202010710897.2A CN202010710897A CN111714465B CN 111714465 B CN111714465 B CN 111714465B CN 202010710897 A CN202010710897 A CN 202010710897A CN 111714465 B CN111714465 B CN 111714465B
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soft capsule
extract
shuangjie
preparation
jiuwei
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CN111714465A (en
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张纯刚
程岚
乔子桐
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Liaoning University of Traditional Chinese Medicine
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Liaoning University of Traditional Chinese Medicine
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    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/4808—Preparations in capsules, e.g. of gelatin, of chocolate characterised by the form of the capsule or the structure of the filling; Capsules containing small tablets; Capsules with outer layer for immediate drug release
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/19—Acanthaceae (Acanthus family)
    • A61K36/195—Strobilanthes
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    • A61K36/23—Apiaceae or Umbelliferae (Carrot family), e.g. dill, chervil, coriander or cumin
    • A61K36/233—Bupleurum
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Abstract

The invention belongs to the field of traditional Chinese medicine preparations and traditional Chinese medicine modernization, and particularly relates to a Jiuwei Shuangjie soft capsule and a preparation method thereof. The nine-ingredient double-effect soft capsule consists of a capsule shell and contents in the capsule shell. The content is a suspension prepared by mixing nine-ingredient double-disintegration extract powder, a dispersion medium, a suspension and a suspending agent; the extract powder is prepared from radix bupleuri, cooked rhubarb, sweet wormwood, honeysuckle, wine-processed radix scutellariae, big green leaves, dandelion, rhizoma paridis and peeled ginger-processed tsaoko cardamom; the capsule shell is made by filling and pressing the suspension into the capsule shell by adopting a rotary film pressing method through gelatin, glycerol and water. The nine-ingredient double-decomposition soft capsule provided by the invention has the advantages of high purity of effective ingredients, environmental-friendly and safe preparation method, easiness in operation and quality control, low cost, effective improvement of the extraction rate of the nine-ingredient double-decomposition preparation, stable performance of the prepared nine-ingredient double-decomposition soft capsule, covering of the uncomfortable taste of the medicine, easiness in swallowing and suitability for large-scale industrial production.

Description

Jiuwei Shuangjie soft capsule and preparation method thereof
Technical Field
The invention belongs to the field of traditional Chinese medicine preparations and traditional Chinese medicine modernization, and relates to a traditional Chinese medicine preparation and a preparation method thereof, in particular to a Jiuwei Shuangjie soft capsule and a preparation method thereof.
Background
The Jiuwei Shuangjie oral liquid is a variety issued by the national drug standard (the new drug trial standard changes to the positive standard). The traditional Chinese medicine is prepared by dialectically treating both symptoms and root causes based on the traditional Chinese medicine theory on the basis of a good formula of Zhongjing fever, namely a large bupleurum decoction and a folk secret formula, namely a famous high-fever decoction, and the whole formula comprises 9 medicines (rheum officinale, honeysuckle, scutellaria baicalensis, dandelion, radix bupleuri, sweet wormwood herb, folium isatidis, rhizoma paridis and amomum tsao-ko), wherein the radix bupleuri is used for relieving exterior syndrome and reducing fever, and the rheum officinale is used for clearing heat and purging pathogenic fire to ensure that pathogenic substances are removed from the exterior and the interior; removing internal heat from sweet wormwood; detoxification of honeysuckle; the scutellaria baicalensis clears heat and dries dampness; besides, the effects of the dyers woad leaf, the dandelion and the paris polyphylla for clearing heat and relieving sore throat are taken; caoguo warms the middle-jiao and eliminates dampness to treat cold of various herbs. The nine materials are used together to play the roles of relieving exterior and interior, clearing heat, purging fire and removing toxicity, and are mainly used for treating wind-heat type common cold caused by external wind-heat type exterior evil, exterior and interior heat type common cold with symptoms of fever or aversion to wind, headache, nasal obstruction, cough, watery nasal discharge, pharyngalgia, thirst, dry stool and the like.
Chinese patent CN201510213827.5 discloses a commercially available jiuwei shuangjie oral liquid, the extraction method of which is: extracting volatile oil from radix bupleuri, sweet wormwood, honeysuckle and amomum tsao-ko by a steam distillation method, soaking the rest of the five medicines of rhubarb, scutellaria, dyers woad leaf, dandelion and rhizoma paridis in 10 times of water, decocting for three times, and extracting effective components. With the method, the leaching rate of effective components is low, impurities are more, and the method is not beneficial to refining and influences the drug effect. The preparation has high requirements on production equipment and process, high cost, special taste and poor patient compliance.
Disclosure of Invention
The invention aims to provide a Jiuwei Shuangjie soft capsule and a preparation method thereof.
The nine-ingredient double-decomposition soft capsule provided by the invention has high purity of effective components, the preparation method effectively improves the extraction rate of the nine-ingredient double-decomposition preparation, is environment-friendly and safe, is easy to operate and carry out quality control, has low cost, has stable performance, covers the uncomfortable taste of the medicine, is easy to swallow, and is suitable for large-scale industrial production.
In order to achieve the above object, the present invention provides the following technical solutions.
A Jiuwei Shuangjie soft capsule comprises the following components: capsule shells and contents within capsule shells.
The content comprises nine-ingredient double-disintegration extract powder, a dispersion medium, a suspension and a suspending agent according to the weight ratio of 10:10-15:0.2:0.5 suspension prepared by mixing.
The extract powder is prepared from the following raw material medicines in parts by weight: 200 parts of radix bupleuri, 140 parts of cooked rhubarb, 200 parts of sweet wormwood herb, 80 parts of honeysuckle, 140 parts of wine-processed radix scutellariae, 155 parts of major green leaves, 140 parts of dandelion, 80 parts of rhizoma paridis and 60 parts of peeled ginger-processed tsaoko amomum fruit.
The capsule shell is prepared from gelatin, glycerol and water according to a weight ratio of 1:0.45:1 in a certain proportion.
The preparation method of the Jiuwei Shuangjie soft capsule specifically comprises the following steps.
Step 1, preparation of Jiuwei Shuangjie extract powder: subjecting bupleuri radix, flos Lonicerae, herba Artemisiae Annuae, fructus Tsaoko, radix et rhizoma Rhei, Scutellariae radix, folium Isatidis, herba Taraxaci, and rhizoma paridis to supercritical CO2Extraction combined with steam distillation, ultrasonic-assisted reflux extraction, and ultrasonicThe microwave-assisted reflux method is used for extracting, concentrating and drying, and the specific preparation method is as follows.
(1) Oven drying bupleuri radix, herba Artemisiae Annuae, flos Lonicerae and fructus Tsaoko at 40 deg.C to constant weight, pulverizing and sieving (20 mesh).
(2) Putting the powder in the step (1) into a supercritical extraction device, and setting CO2The flow rate is 2.5Lg/min, the pressure of an extraction kettle is 35MPa, the pressure of a separation kettle I is 20MPa and 40 ℃, the pressure of a separation kettle II is 12MPa and 25 ℃, and the extract is collected from the opening of the separation kettle for standby after the volume of the volatile oil is not increased any more; and adding water to dissolve the residue, wherein the material-liquid ratio is 1:50(g: ml), extracting by steam distillation (temperature not higher than 80 deg.C) until the volume of volatile oil is not increased, and mixing.
(3) Taking rhubarb, scutellaria baicalensis and rhizoma paridis according to a material-liquid ratio of 1: adding 80% ethanol into 30g (ml), ultrasonic extracting at 60 deg.C (55KHz,250W) for 35min, reflux extracting for 1.5h, filtering, and recovering ethanol.
(4) Oven drying folium Isatidis and herba Taraxaci at 60 deg.C to constant weight. Pulverizing, sieving (40 mesh), adding 60% ethanol at a material-to-liquid ratio of 1:20(g: ml), heating to 65 deg.C in ultrasonic-microwave synergistic extraction apparatus, fixing microwave power of 100W and ultrasonic power of 200W, reflux extracting for 1.5 hr, filtering, and recovering ethanol.
(5) And (3) mixing the solution in the step (3) and the solution in the step (4), uniformly mixing, and concentrating to obtain an extract with the relative density of 1.10-1.30 (75 ℃).
(6) Uniformly mixing the extract in the step (5) with the volatile oil in the step (2), and adding soluble starch according to a certain weight ratio of the extract amount when the extract is hot: soluble starch 25:1, stirring, spray-drying and crushing into 120-mesh powder to obtain the Jiuwei Shuangjie extract powder.
Step 2, preparing the soft capsule: taking gelatin, glycerol and water according to a ratio, and filling and pressing the suspension into a capsule shell by adopting a rotary film pressing method to prepare the soft capsule.
(1) The nine-ingredient double-disintegration extract powder is uniformly mixed with soybean oil, soybean lecithin and beeswax according to the proportion to prepare a suspension for later use.
(2) According to the weight ratio of 1:0.45:1, taking gelatin, glycerol and water, boiling the gelatin, removing bubbles under reduced pressure, and filter-pressing the gelatin to a gelatin storage tank for heat preservation at 60 ℃ for later use.
(3) And (3) filling and pressing the suspension in the step (1) to the capsule shell in the step (2) through a rotary film pressing method to prepare a soft capsule, shaping at the temperature of below 18-25 ℃, wiping off an oil layer on the surface of the soft capsule by using a non-fiber rag, and drying at the temperature of below 28 ℃ to obtain the nine-ingredient double-effect soft capsule.
Compared with the prior art, the invention has the following beneficial effects.
(1) The preparation method of the nine-ingredient double-effect soft capsule uses supercritical CO2The extraction and steam distillation method maximally retain the volatile oil in bupleuri radix, herba Artemisiae Annuae, flos Lonicerae and fructus Tsaoko, shorten extraction time, and reduce energy consumption and pollution.
(2) The preparation method of the Jiuwei Shuangjie soft capsule provided by the invention adopts an ultrasonic-assisted reflux extraction method to treat the rhubarb, the scutellaria baicalensis and the rhizoma paridis, so that the yield is greatly improved, the energy consumption is low, the extraction time is short, and the economic benefit is higher.
(3) The preparation method of the Jiuwei Shuangjie soft capsule provided by the invention treats dandelion and folium isatidis by using an ultrasonic-microwave assisted reflux method, destroys plant cell walls and intercellular substance, accelerates the dissolution rate of effective components, improves the efficiency, shortens the time, reduces the dosage of solvent and reduces the cost.
(4) The Jiuwei Shuangjie soft capsule provided by the invention has the advantages of high content of effective components, good stability, light carrying and convenient use. And the bad smell of the nine-ingredient double-effect oral liquid is covered, and the compliance of patients is improved.
Detailed Description
The technical scheme and the technical effect of the invention are described in detail by combining specific embodiments. The following examples are only preferred embodiments of the present invention, and are not intended to limit the present invention, and it will be apparent to those skilled in the art that various changes and modifications can be made in the present invention, and any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
A Jiuwei Shuangjie soft capsule comprises the following components: capsule shells and contents within capsule shells.
The content is a suspension prepared by mixing nine-ingredient double-disintegration extract powder, a dispersion medium, a suspension and a suspending agent according to the weight ratio of 10:10-15:0.2: 0.5.
The extract powder is prepared from the following raw material medicines in parts by weight: 200 parts of radix bupleuri, 140 parts of cooked rhubarb, 200 parts of sweet wormwood herb, 80 parts of honeysuckle, 140 parts of wine-processed radix scutellariae, 155 parts of major green leaves, 140 parts of dandelion, 80 parts of rhizoma paridis and 60 parts of peeled ginger-processed tsaoko amomum fruit.
The capsule shell is prepared by filling and pressing the suspension into the capsule shell by a rotary film pressing method according to the weight ratio of gelatin, glycerol and water of 1:0.45: 1.
The preparation method of the Jiuwei Shuangjie soft capsule is shown in the first embodiment to the third embodiment.
Example one.
The preparation method of the Jiuwei Shuangjie soft capsule specifically comprises the following steps.
(1) Taking 2.0kg of radix bupleuri, 2.0kg of sweet wormwood herb, 0.8kg of honeysuckle flower and 0.6kg of tsaoko cardamom, drying the materials in a drying oven at 40 ℃ until the weight is constant, crushing and sieving the materials by a sieve of 20 meshes.
(2) Putting the powder in the step (1) into a supercritical extraction device, and setting CO2Extracting at a flow rate of 2.5L/min and an extraction kettle pressure of 35MPa, a separation kettle I pressure of 20MPa, a separation kettle I pressure of 12MPa and a separation kettle II pressure of 25 ℃ until the volume of the volatile oil is not increased any more, and collecting the extract from the opening of the separation kettle for later use; dissolving the residue in water at a ratio of 1:50(g: ml), extracting by steam distillation (at a temperature of no more than 80 deg.C) until the volume of volatile oil is not increased, and mixing.
(3) Adding appropriate amount of 80% ethanol into radix et rhizoma Rhei 1.4kg, Scutellariae radix 1.4kg, and rhizoma paridis 0.8kg, performing ultrasonic extraction at 60 deg.C (55KHz,250W) for 35min, reflux-extracting for 1.5 hr, filtering, and recovering ethanol.
(4) 1.55kg of dyers woad leaf and 1.4kg of dandelion are dried in an oven at 60 ℃ to constant weight. Pulverizing, sieving (40 mesh), adding 60% ethanol, heating to 65 deg.C in ultrasonic-microwave synergistic extraction apparatus, fixing microwave power of 100W and ultrasonic power of 200W, reflux extracting for 1.5 hr, filtering, and recovering ethanol.
(5) And (3) mixing the solution in the step (3) and the solution in the step (4), uniformly mixing, and concentrating to obtain an extract with the relative density of 1.18(75 ℃).
(6) Uniformly mixing the extract in the step (5) with the volatile oil in the step (2), and adding soluble starch according to a certain weight ratio of the extract amount when the extract is hot: soluble starch 25:1, stirring, spray-drying and crushing into 120-mesh extract powder.
(7) According to the weight ratio, the nine-ingredient double-disintegration extract powder is uniformly mixed with soybean oil, soybean lecithin and beewax according to the ratio of 10:15:1:2 to prepare a suspension for later use.
(8) Taking gelatin, glycerol and water according to the weight ratio of 1:0.45:1, boiling the gelatin, removing bubbles under reduced pressure, and performing filter pressing to a gelatin storage tank for keeping the temperature at 60 ℃ for later use.
(9) And (3) performing filling and pressing on the suspension in the step (7) to the capsule shell in the step (8) by a rotary film pressing method to prepare soft capsules, forming at the temperature of below 25 ℃, wiping off an oil layer on the surfaces of the soft capsules by using a non-fiber rag, and drying at the temperature of below 28 ℃ to obtain 10000 Jiuwei Shuangjie soft capsules.
Example two.
The preparation method of the Jiuwei Shuangjie soft capsule specifically comprises the following steps.
(1) Taking 200g of radix bupleuri, 200g of sweet wormwood herb, 80g of honeysuckle flower and 60g of tsaoko amomum fruit, drying the materials in a 40 ℃ oven until the weight is constant, crushing and sieving the materials by a sieve (20 meshes).
(2) Putting the powder in the step (1) into a supercritical extraction device, and setting CO2The flow rate is 2.5Lg/min, the pressure of an extraction kettle is 35MPa, the pressure of a separation kettle I is 20MPa, the temperature of a separation kettle I is 40 ℃, the pressure of a separation kettle II is 12MPa, the temperature is 25 ℃, extraction is carried out until the volume of the volatile oil is not increased any more, and an extract is collected from the opening of the separation kettle for later use; dissolving the residue in water at a ratio of 1:50(g: ml), extracting by steam distillation (temperature not higher than 80 deg.C) until the volume of volatile oil is not increased, and mixing.
(3) Adding appropriate amount of 80% ethanol into 140g of radix et rhizoma Rhei, 140g of Scutellariae radix and 80g of rhizoma paridis, performing ultrasonic treatment at 60 deg.C (55KHz,250W) for 35min, reflux-extracting for 1.5h, filtering, and recovering ethanol.
(4) 155g of dyers woad leaf and 140g of dandelion are dried in an oven at 60 ℃ until the weight is constant. Pulverizing, sieving (40 mesh), adding 60% ethanol, heating to 65 deg.C in ultrasonic-microwave synergistic extraction apparatus, fixing microwave power of 100W and ultrasonic power of 200W, reflux extracting for 1.5 hr, filtering, and recovering ethanol.
(5) And (3) mixing the solution in the step (3) and the solution in the step (4), uniformly mixing, and concentrating to obtain an extract with the relative density of 1.18(75 ℃).
(6) Uniformly mixing the extract in the step (5) with the volatile oil in the step (2), and adding soluble starch according to a certain weight ratio of the extract amount when the extract is hot: soluble starch 25:1, stirring, spray-drying and crushing into 120-mesh extract powder.
(7) Mixing the Jiuwei Shuangjie extract powder, the soybean oil, the soybean lecithin and the beewax according to the weight ratio of 10:10:0.2:0.5 to prepare a suspension for later use.
(8) Taking gelatin, glycerol and water according to the weight ratio of 1:0.45:1, boiling the gelatin, and filter-pressing the gelatin to a gelatin storage tank for heat preservation at 60 ℃ for later use.
(9) And (3) filling and pressing the suspension in the step (7) to the capsule shell in the step (8) through a rotary film pressing method to prepare a soft capsule, shaping at the temperature of below 20 ℃, wiping off an oil layer on the surface of the soft capsule by using a fiber-free rag, and drying at the temperature of below 28 ℃ to obtain 1000 Jiuwei Shuangjie soft capsules.
Example three.
The preparation method of the Jiuwei Shuangjie soft capsule specifically comprises the following steps.
(1) Taking 330g of radix bupleuri, 330g of sweet wormwood, 130g of honeysuckle and 100g of tsaoko amomum fruit, drying the materials in a 40 ℃ oven until the weight is constant, crushing and sieving the materials by a sieve (20 meshes).
(2) Putting the powder in the step (1) into a supercritical extraction device, and setting CO2Extracting at a flow rate of 2.5L/min and an extraction kettle pressure of 35MPa, a separation kettle I pressure of 20MPa, a separation kettle I pressure of 12MPa and a separation kettle II pressure of 25 ℃ until the volume of the volatile oil is not increased any more, and collecting the extract from the opening of the separation kettle for later use; dissolving the residue in water at a ratio of 1:50(g: ml), extracting by steam distillation (temperature not higher than 80 deg.C) until the volume of volatile oil is not increased, and mixing.
(3) Adding appropriate amount of 80% ethanol into 230g of radix et rhizoma Rhei, 230g of Scutellariae radix and 130g of rhizoma paridis, performing ultrasonic treatment at 60 deg.C (55KHz,250W) for 35min, reflux-extracting for 1.5h, filtering, and recovering ethanol.
(4) And (3) drying 255g of folium isatidis and 230g of dandelion in an oven at 60 ℃ until the weight is constant. Pulverizing, sieving (40 mesh), adding 60% ethanol, heating to 65 deg.C in ultrasonic-microwave synergistic extraction apparatus, fixing microwave power of 100W and ultrasonic power of 200W, reflux extracting for 1.5 hr, filtering, and recovering ethanol.
(5) And (3) mixing the solution in the step (3) and the solution in the step (4), uniformly mixing, and concentrating to obtain an extract with the relative density of 1.18(75 ℃).
(6) And (3) uniformly mixing the extract in the step (5) and the volatile oil in the step (2), and adding soluble starch according to the amount of the extract in a certain weight ratio when the extract is hot: soluble starch 25:1, stirring, spray drying, and pulverizing into 120 mesh extract powder.
(7) Mixing the Jiuwei Shuangjie extract powder, the soybean oil, the soybean lecithin and the beewax according to the weight ratio of 10:10:0.2:0.5 to prepare a suspension for later use.
(8) Taking gelatin, glycerol and water according to the weight ratio of 1:0.45:1, boiling the gelatin, removing bubbles under reduced pressure, and performing filter pressing to a gelatin storage tank for keeping the temperature at 60 ℃ for later use.
(9) And (3) filling and pressing the suspension in the step (8) to the capsule shell in the step (9) through a rotary film pressing method to prepare a soft capsule, shaping at 23 ℃, wiping off an oil layer on the surface of the soft capsule by using a fiber-free rag, and drying at the temperature of below 28 ℃ to obtain the nine-ingredient double-effect soft capsule.
Example four determination of content of effective components in soft capsules and oral liquid.
1. Functional components and indexes.
According to the national medicine standard WS3-641(Z-091) -2004(Z), the Jiuwei Shuangjie oral liquid contains rheum officinale (C) and emodin (C) in each 1ml15H10O5) In terms of content, the content should not be less than 0.095 mg. Therefore, like the Jiuwei Shuangjie oral liquid, the effective component of the product is emodin.
2. Measuring the content of effective components in the soft capsule and the oral liquid.
(1) The content of emodin in the product and the Jiuwei Shuangjie oral liquid is determined by an HPLC method.
The chromatographic conditions are as follows: a chromatographic column: dikma Diamond C18(200 mm. times.4.6 mm; 5 μm); flow ofMoving phase: methanol-water-0.1% phosphoric acid solution (80:20: 0.02); flow rate: 0.8 ml/min-1(ii) a Column temperature: 30 ℃; sample introduction amount: 10 mu L of the solution; detection wavelength: 290 nm.
(2) Standard curve determination and sample processing methods.
Accurately weighing appropriate amount of emodin reference substance, and adding methanol to obtain 1ml reference substance solution containing emodin 0.1 mg. Precisely absorbing the solution into 2, 4, 6, 8 and 10mL to 10mL volumetric flasks respectively, diluting with methanol to scale, shaking up, absorbing 10 microliter respectively, injecting into a high performance liquid chromatograph for determination, and taking peak area A as a vertical coordinate and concentration C (microgram/mL) of emodin as a horizontal coordinate to obtain a standard curve equation: Y4387062.146X-7162.7139 and r 0.99998.
Taking about 0.3g of the content of the product, precisely weighing, placing in a 100mL volumetric flask, adding 60mL of methanol for dissolving, carrying out ultrasonic treatment for 30min, and then fixing the volume to the scale with the methanol. Precisely absorbing 5mL of the solution, placing the solution in a 10mL volumetric flask, diluting the solution to the scale with methanol, shaking up, absorbing 10 mu L of the solution, injecting the solution into a high performance liquid chromatograph to measure the peak area, and calculating the content of the emodin of the variety according to a standard curve.
Precisely measuring 10mL of the nine-ingredient double-effect oral liquid, placing the nine-ingredient double-effect oral liquid into a 100mL volumetric flask, diluting the nine-ingredient double-effect oral liquid to a scale with methanol, sucking 10 mu L of the nine-ingredient double-effect oral liquid, injecting the nine-ingredient double-effect oral liquid into a high performance liquid chromatograph to measure peak area, and calculating the content of emodin in the nine-ingredient double-effect oral liquid according to a standard curve.
(3) The results are shown in Table 1.
Table 1. results of determination of emodin content in jiuwei dujie oral liquid and examples one to three.
Figure BDA0002596501290000071
The results show that compared with the Jiuwei Shuangjie oral liquid, the content of the emodin in the soft capsule prepared by the invention is obviously improved.
Example five nine ingredients double-effect soft capsule preparation method process screening experiments.
First, the experiment of comparing effect of supercritical extraction combined with steam distillation method and steam distillation method.
1. And (3) preparing the volatile oil.
Supercritical extraction combined with steam distillation: extracting volatile oil according to the operation steps of (2) in the first to third examples respectively, and calculating the oil extraction rate.
Steam distillation method: samples were prepared according to the procedure (1) in examples one to three, respectively, and dissolved in water at a ratio of 1:50(g: ml) in a steam distillation apparatus (temperature controlled not to exceed 80 ℃) until the volatile oil did not increase, fractions were collected, and the oil extraction rate was calculated.
Oil extraction rate (M)1/M2) X 100%, wherein M1Is the mass (g) of volatile oil; m2Is the sample mass (g).
2. The results are shown in Table 2.
Table 2. comparing the volatile oil extraction rate by combining the supercritical extraction with the steam distillation method.
Figure BDA0002596501290000072
The results show that compared with the steam distillation method, the yield of the volatile oil extracted by combining the supercritical extraction with the steam distillation method is improved by 11 times, the extraction time is shortened from 20h to 5h, and the energy consumption is reduced.
And II, screening experiments of the extraction method.
Comparing the extraction effects of the ultrasonic-assisted reflux extraction method, the microwave-assisted reflux extraction method and the decoction method on the rhubarb, the scutellaria baicalensis and the rhizoma paridis.
After the rhubarb, the baicalin and the rhizoma paridis medicinal materials are crushed and properly processed (including a decoction method, an ultrasonic-assisted reflux extraction method and a microwave-assisted reflux extraction method), the transfer rates of the emodin, the baicalin and the rhizoma paridis saponin are respectively used as indexes, and the difference among the extraction methods is compared.
1. And (4) a treatment method.
The decocting method comprises the following steps: respectively taking 50.00g of the three powders, adding 10 times of ultrapure water for soaking for 1h, decocting and extracting for 2 times, 1h each time, filtering with gauze, and concentrating the filtrate.
Microwave-assisted reflux extraction: weighing 50.00g of 40-mesh radix Scutellariae powder, adding 80% ethanol according to a material-liquid ratio of 1:30(g: ml), performing microwave treatment at power of 650W for 35min, reflux-extracting for 1.5h, filtering, recovering ethanol, and concentrating for use.
Ultrasonic assisted-reflux extraction method: respectively taking 50.00g of each of the three powders, adding 80% ethanol according to a material-liquid ratio of 1:30(g: ml), performing ultrasonic treatment (55KHz,250W) at 60 ℃ for 35min, performing reflux extraction for 1.5h, filtering, recovering ethanol, and concentrating for later use.
2. And (5) measuring a standard curve.
Rhubarb: 20mg of the emodin standard substance is precisely weighed and placed in a 1000ml volumetric flask, and then dissolved in methanol, and the volume is determined to the scale. Precisely sucking 1mL, 2mL, 3mL, 4mL and 5mL, respectively placing in a 10mL measuring flask, adding 0.5% magnesium acetate-methanol solution to the scale, and standing for 20 min. The absorbance of the solution at 510nm was measured in each case using a 0.5% magnesium acetate-methanol solution as a blank. Standard curves were plotted as absorbance versus concentration, Y0.07431X +0.01538, r 0.99998.
Scutellaria baicalensis: accurately weighing 20.00mg of baicalin standard substance, accommodating the baicalin standard substance in a 1000mL volumetric flask by absolute ethyl alcohol, accurately sucking 1mL, 2mL, 3mL, 4mL and 5mL, accommodating the baicalin standard substance in a 50mL volumetric flask by absolute ethyl alcohol, measuring the absorbance of the baicalin at 278nm by taking the absorbance A as a vertical coordinate and taking the mass concentration (mu g/mL) of the baicalin standard solution as a horizontal coordinate, and drawing a standard curve, wherein Y is 0.10349X +0.01761, and r is 0.99997.
Rhizoma paridis: accurately weighing 20.00mg of the paris polyphylla saponin standard substance, fixing the volume in a 1000mL volumetric flask by using methanol, accurately sucking 1mL, 2mL, 3mL, 4mL and 5mL, fixing the volume in a 50mL volumetric flask by using methanol, measuring the absorbance at 415nm, taking the value A as the ordinate and the corresponding paris polyphylla saponin standard substance concentration (mu g/mL) as the abscissa, and drawing a standard curve, wherein Y is 48.72251X +0.10739, and r is 0.99993.
3. A sample processing method.
Rhubarb: adding 2.5mol/L sulfuric acid 20ml into the treated concentrate, hydrolyzing for 2h, slightly cooling, adding chloroform 20ml, transferring into a separating funnel, taking a chloroform layer, continuously extracting an acid water layer with chloroform for 3 times, combining, precisely absorbing 30ml, washing with distilled water to be neutral, putting on a water bath to volatilize the chloroform layer, dissolving the residue with 0.5% magnesium acetate-methanol solution, fixing the volume to a 10ml volumetric flask, shaking up, standing for 20min, measuring the absorbance value at 510nm by using an ultraviolet spectrophotometry method, and calculating the emodin content.
Scutellaria baicalensis: and (3) using a hydrochloric acid solution with the mass fraction of 10% to the treated concentrate, adjusting p H-2.0 of the filtrate, standing in a water bath at the temperature of 80 ℃, using absolute ethyl alcohol to pump and wash the precipitate for 2-3 times, and drying to obtain a baicalin crude extract. Measuring the absorbance value of the baicalin by using an ultraviolet-visible spectrophotometer at the wavelength of 278nm, and calculating the baicalin content.
Rhizoma paridis: adding water saturated n-butanol into the treated concentrate, measuring its absorbance value at 415nm wavelength with ultraviolet-visible spectrophotometer, and calculating the content of rhizoma paridis saponin.
4. The results are shown in Table 3.
TABLE 3 different extraction methods for rhubarb, baikal skullcap root and paris rhizome.
Figure BDA0002596501290000091
The results show that the ultrasonic extraction method has better extraction effect than the decoction method and the microwave method.
And thirdly, comparing the extraction effects of the decocting method and the ultrasonic-microwave assisted reflux method on the dyers woad leaf and the dandelion.
After the folium isatidis and the dandelion are ground and appropriately treated (including a decoction method and an ultrasonic-microwave assisted reflux method), the transfer rates of indirubin and caffeic acid are respectively used as indexes, and the difference between the extraction methods is compared.
1. And (4) a treatment method.
The decocting method comprises the following steps: respectively taking 50.00g of the two kinds of powder, adding ultrapure water with the volume of 10 times, soaking for 1h, decocting and extracting for 2 times, each time for 1h, filtering by gauze, and concentrating the filtrate.
An ultrasonic-microwave assisted reflux method: respectively taking 50.00g of each of the two powders, adding a proper amount of 60% ethanol, putting the two powders into an ultrasonic-microwave synergistic extraction instrument to 65 ℃, fixing the microwave power of 100W and the ultrasonic power of 200W, carrying out reflux extraction for 1.5h, filtering, recovering ethanol, and concentrating for later use.
2. Chromatographic conditions.
Folium isatidis: a chromatographic column: agilent HC-C18 (4.6X 250mm, 5 μm) with methanol-water (75:25) as the mobile phase; the column temperature is 30 ℃; the flow rate is 1.0 mL/min; the detection wavelength is 289 nm.
Dandelion: a chromatographic column: agilent HC-C18 (4.6X 250mm, 5 μm); the mobile phase is methanol-0.1% phosphoric acid water solution (25: 75); the column temperature is 30 ℃; the flow rate is 1.0 mL/min; the detection wavelength 323 mm.
3. And (5) measuring a standard curve.
Folium isatidis: accurately weighing 20.00mg of indirubin standard substance, fixing the volume in a 1000mL volumetric flask by using methanol, accurately sucking 1mL, 2mL, 3mL, 4mL and 5mL, fixing the volume in a 50mL volumetric flask by using methanol, fixing the volume to a scale by using methanol to obtain 6 reference substance solutions with different concentrations, respectively injecting 20 mu L of reference substance solutions, determining peak areas by using a high performance liquid chromatograph, and drawing a standard curve by using the concentration as an abscissa and the peak area as an ordinate, wherein Y is 18.86003x +38.75421, and r is 0.99993.
Dandelion: precisely sucking 20.00mg of caffeic acid standard substance, fixing the volume with methanol in a 1000mL volumetric flask, precisely sucking 1mL, 2mL, 3mL, 4mL and 5mL, fixing the volume with methanol in a 50mL volumetric flask, fixing the volume with methanol to a scale to obtain 6 reference substance solutions with different concentrations, sucking 20 μ L, injecting into a high performance liquid chromatograph, and drawing a standard curve by taking the concentration as an abscissa and the peak area as an ordinate as a measurement peak area, wherein Y is 63.67064X-0.25429, and r is 0.99998.
4. A sample processing method.
Respectively weighing 0.3g of two medicinal material concentrates prepared by different treatment methods, precisely weighing, placing in a 100mL volumetric flask, adding 60mL of methanol for dissolving, ultrasonically treating for 30min, and fixing the volume to the scale with methanol. Precisely sucking 5mL of the solution, placing the solution in a 10mL volumetric flask, diluting the solution to a scale with methanol, shaking up, sucking 20 mu L of the solution, injecting the solution into a high performance liquid chromatograph to measure peak area, and calculating the content of indirubin and caffeic acid according to the standard curves of the two solutions.
5. The results are shown in Table 4.
TABLE 4. different extraction methods for folium Isatidis and herba Taraxaci.
Figure BDA0002596501290000101
The results show that the ultrasonic-microwave assisted reflux method has better extraction effect than the decoction method.
Example six nine ingredient double-effect soft capsules were examined for disintegration time and stability.
1. And (5) inspecting disintegration time limit.
Taking the first to third examples as samples, taking 6 granules respectively, placing the samples into a lifting disintegration tester for inspection, and placing artificial gastric juice in a beaker at the temperature of 37 ℃. The soft capsules prepared in the examples one to three all meet the standard through detection. The results of the experiments are shown in Table 5.
Table 5. examples one to three disintegration time measurements (n ═ 6).
Figure BDA0002596501290000111
2. And (5) stability inspection.
Taking the first to third examples as the test samples, taking three batches of the test samples respectively, placing the three batches of the test samples for 12 months under the conditions of the temperature of 25 +/-2 ℃ and the relative humidity of 60 +/-5%, and periodically inspecting the changes of the preparation properties, the disintegration time limit and the emodin content. The results show that after 12 months, the preparation has no adhesion, no leakage and no precipitation of the content, the content reduction ratio is 1.40% at the lowest, the reduction is only 2.34% at the highest, the stability is good, and the results are shown in Table 6.
Table 6 stability studies of examples one to three.
Figure BDA0002596501290000112
In conclusion, the Jiuwei Shuangjie soft capsule prepared by the invention has high extraction rate, good stability and low energy consumption, and is suitable for industrial production.

Claims (1)

1. The preparation method of the Jiuwei Shuangjie soft capsule is characterized by comprising the following steps:
step 1, preparation of Jiuwei Shuangjie extract powder:
(1) drying bupleuri radix, herba Artemisiae Annuae, flos Lonicerae and fructus Tsaoko at 40 deg.C in oven to constant weight, pulverizing, and sieving with 20 mesh sieve;
(2) putting the powder prepared in the step (1) into a supercritical extraction device, and setting CO2The flow rate is 2.5Lg/min, the pressure of an extraction kettle is 35MPa, the pressure of a separation kettle I is 20MPa and 40 ℃, the pressure of a separation kettle II is 12MPa and 25 ℃, and the extract is collected from the opening of the separation kettle for standby after the volume of the volatile oil is not increased any more; and adding water to dissolve the residue, wherein the material-liquid ratio is 1:50(g: mL), extracting by steam distillation at a temperature not higher than 80 deg.C until the volume of volatile oil is not increased, and mixing;
(3) taking rhubarb, scutellaria and rhizoma paridis according to a material-liquid ratio of 1: adding 80% ethanol into 30(g: mL), performing ultrasonic treatment at 60 deg.C under 55KHz for 35min under 250W, reflux extracting for 1.5h, filtering, and recovering ethanol;
(4) drying folium Isatidis and herba Taraxaci in a 60 deg.C oven to constant weight, pulverizing, sieving with 40 mesh sieve, adding appropriate amount of 60% ethanol according to a material-liquid ratio of 1:20(g: mL), heating to 65 deg.C in an ultrasonic-microwave synergistic extraction apparatus, fixing microwave power of 100W and ultrasonic power of 200W, reflux extracting for 1.5h, filtering, and recovering ethanol;
(5) mixing the solution prepared in the step (3) and the solution prepared in the step (4), uniformly mixing, and concentrating to obtain an extract with the relative density of 1.10-1.30 (75 ℃);
(6) uniformly mixing the extract in the step (5) with the volatile oil in the step (2), and adding soluble starch according to a certain weight ratio of the extract amount when the extract is hot: soluble starch = 25:1, stirring, spray-drying, and crushing into 120-mesh powder to obtain nine-ingredient Shuangjie extract powder;
step 2, preparing the soft capsule:
(1) mixing the above nine-ingredient double-decomposition extract powder with soybean oil, soybean phospholipid and Cera flava uniformly according to a ratio to obtain suspension;
(2) according to the weight ratio of 1:0.45:1, taking gelatin, glycerol and water according to the proportion, boiling the gelatin, removing bubbles under reduced pressure, and performing filter pressing on the gelatin to a gelatin storage tank for keeping the temperature at 60 ℃ for later use;
(3) and (3) filling and pressing the suspension in the step (1) into the capsule shell prepared in the step (2) by a rotary film pressing method to prepare a soft capsule, shaping at the temperature of below 18-25 ℃, wiping off an oil layer on the surface of the soft capsule by using a non-fiber rag, and drying at the temperature of below 28 ℃ to obtain the nine-ingredient double-effect soft capsule.
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CN104771687A (en) * 2015-04-30 2015-07-15 吉林恒金药业股份有限公司 Application of Jiu Wei Shuang Jie Kou Fu Ye to prepare drug for treating chronic hepatitis

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