阅读说明：本技术 一种银黄颗粒的制备方法 (Preparation method of honeysuckle flower and scutellaria baicalensis granules ) 是由 曾英姿 周万辉 赵磊 于 2020-12-31 设计创作，主要内容包括：本发明涉及一种银黄颗粒的制备方法,所述方法包括以下步骤：步骤1.取金银花,以水为提取溶媒,提取三次,药液浓缩,干燥得金银花提取物；步骤2.取黄芩,以水为提取溶媒,提取二次,煎液滤过,药渣备用；步骤3.滤液浓缩,加入乙醇使溶液中乙醇含量为60-80％,静置,过滤,回收乙醇并浓缩得到水提浸膏；步骤4.药渣用乙醇回流提取二次,提取液滤过,回收乙醇并浓缩得醇提浸膏；步骤5.合并水提浸膏与醇提浸膏,干燥即得黄芩提取物；步骤6.将金银花提取物、黄芩提取物、药用糊精、甜菊素混合均匀,进行制粒,得到银黄颗粒。(The invention relates to a preparation method of Yinhuang granules, which comprises the following steps: step 1, taking honeysuckle, extracting for three times by taking water as an extraction solvent, concentrating the liquid medicine, and drying to obtain a honeysuckle extract; step 2, taking the scutellaria baicalensis, extracting twice by taking water as an extraction solvent, filtering decoction liquid, and reserving dregs for later use; step 3, concentrating the filtrate, adding ethanol to ensure that the ethanol content in the solution is 60-80%, standing, filtering, recovering ethanol and concentrating to obtain water extract; step 4, refluxing and extracting the dregs of a decoction twice by using ethanol, filtering an extracting solution, recovering the ethanol and concentrating to obtain an ethanol extract; step 5, combining the water extract and the alcohol extract, and drying to obtain the scutellaria baicalensis extract; and 6, uniformly mixing the honeysuckle extract, the scutellaria baicalensis extract, the medicinal dextrin and the steviosin, and granulating to obtain the honeysuckle-scutellaria baicalensis granules.)

1. A preparation method of Yinhuang granules comprises the following steps: 60-140 parts of honeysuckle extract, 20-60 parts of scutellaria extract, 200-400 parts of medicinal dextrin and 3.0-5.0 parts of steviosin;

the preparation method comprises the following steps:

step 1, taking honeysuckle, extracting for three times by taking water as an extraction solvent, concentrating the liquid medicine, and drying to obtain a honeysuckle extract;

step 2, taking the scutellaria baicalensis, extracting twice by taking water as an extraction solvent, filtering decoction liquid, and reserving dregs for later use;

step 3, concentrating the filtrate, adding ethanol to ensure that the ethanol content in the solution is 60-80%, standing, filtering, recovering ethanol and concentrating to obtain water extract;

step 4, refluxing and extracting the dregs of a decoction twice by using ethanol, filtering an extracting solution, recovering the ethanol and concentrating to obtain an ethanol extract;

step 5, combining the water extract and the alcohol extract, and drying to obtain the scutellaria baicalensis extract;

and 6, uniformly mixing the honeysuckle extract, the scutellaria baicalensis extract, the medicinal dextrin and the steviosin, and granulating to obtain the honeysuckle-scutellaria baicalensis granules.

2. The method of claim 1, wherein the Yinhuang granules are formulated as: 100 parts of honeysuckle extract, 40 parts of scutellaria extract, 300 parts of medicinal dextrin and 4 parts of steviosin;

the preparation method comprises the following steps:

step 1, extracting honeysuckle for three times by taking water as an extraction solvent, wherein the water adding amount is respectively 12 times, 8 times and 7 times, the concentration temperature is 40-70 ℃, the vacuum degree is 0.04-0.08, the concentration time is 8-10 hours, the drying temperature is 70-80 ℃, the vacuum degree is 0.06-0.08, and the drying time is 15-16 hours, so that the honeysuckle extract is obtained;

step 2, extracting the scutellaria baicalensis for 2 times by taking water as an extraction solvent, wherein the amount of water added for each time is 10 times and 6 times, decocting for 2 hours each time, filtering decoction, and reserving dregs for later use;

step 3, merging the filtrates, concentrating until the relative density is 1.05, adding 95% ethanol to ensure that the ethanol content in the solution is 70%, standing for 12 hours, filtering to obtain a supernatant, recovering the ethanol, and concentrating until a water extract with the relative density of 1.25 is obtained;

step 4, reflux-extracting the dregs of a decoction for 2 times by using 95% (V/V) ethanol, wherein the water addition amount is 8 times and 6 times of that of each time, reflux-extracting for 2 hours each time, filtering the extracting solution, combining the filtrates, recovering the ethanol, and concentrating the ethanol to obtain an ethanol extract with the relative density of 1.15;

step 5, combining the water extract and the alcohol extract, drying under reduced pressure at 80-90 ℃ under a vacuum degree of 0.06-0.08 for 6-10 hours to obtain the scutellaria baicalensis extract;

and 3, uniformly mixing 2.4g of honeysuckle extract (calculated as chlorogenic acid), 24g of scutellaria extract (calculated as baicalin), medicinal dextrin and stevioside, and granulating to obtain the Yinhuang granules.

Technical Field

The invention relates to preparation of a medicinal preparation, in particular to a preparation method of traditional Chinese medicine Yinhuang granules.

Background

The Yinhuang granules are a Chinese patent medicine with the efficacies of clearing heat, dispelling wind, relieving sore throat and detoxifying, are composed of honeysuckle extract and scutellaria extract, have the main components of chlorogenic acid and baicalin, are used for treating acute and chronic tonsillitis, acute and chronic pharyngolaryngitis and upper respiratory tract infection, and are widely applied clinically.

The preparation method of the Yinhuang granules disclosed in pharmacopoeia of 2000 comprises the following steps: the formula is as follows: 100g of honeysuckle extract, 40g of scutellaria extract and more than two medicines (preparation method), adding 800g of cane sugar and a proper amount of starch, crushing into fine powder, mixing uniformly, preparing into granules, drying at the temperature of below 60 ℃, and preparing into 1000 g; or adding dextrin and appropriate amount of aspartame, mixing, granulating, drying at 60 deg.C below, and making into 1000g (no sucrose) granule, 4g per bag. The above honeysuckle flower extract per bag of the above honeysuckle flower granule is calculated by chlorogenic acid (C16H18O9), and should not be less than 5.0 mg; the content of Scutellariae radix extract in each bag is not less than 122mg calculated as baicalin (C21H18O 11).

The preparation method of the Yinhuang granules disclosed in the pharmacopoeia of 2015 comprises the following steps: honeysuckle extract (calculated by chlorogenic acid) 2.4g and scutellaria root extract (calculated by baicalin) 24g, and its preparation method includes adding sucrose 480g [1], mixing with proper quantity of starch, pulverizing into fine powder, uniformly mixing them, granulating, drying at 60 deg.C or below to obtain 600g [2], or adding dextrin and proper quantity of protein sugar (or 50% -60% steviosin alcohol solution), uniformly mixing them, granulating, drying at 60 deg.C or below to obtain 300g (without sucrose). The content of flos Lonicerae extract in each bag is not less than 13.6-18.4 mg calculated by chlorogenic acid (C16H18O 9). Each bag of the product contains 136-184 mg of baicalin (C21H18O11) as an extract of radix Scutellariae. It is administered after mixing with boiling water. 1-2 bags at a time, 2 times a day.

The inventor finds that the honeysuckle and scutellaria granules prepared by the prior art are unstable under the condition of high humidity or long-term storage, and the content of active ingredients such as chlorogenic acid, baicalin, wogonoside, wogonin and oroxylin A is reduced or even does not reach the standard in terms of active ingredients.

Disclosure of Invention

The invention provides a honeysuckle and scutellaria baicalensis medicinal composition which is prepared from the following Chinese medicinal raw materials in parts by weight:

the invention aims to overcome the defects in the prior art and provide the Yinhuang granules and the preparation method thereof.

The inventor notices that although the pharmacopoeia is listed in the prior art, the pharmacopoeia only limits the amount of effective components in the extract, the preparation method and the source of the extract are not limited, so that the difference exists between the purchased extracts produced by different manufacturers, which is probably caused by different extraction modes, and therefore, the inventor researches the extraction modes of the honeysuckle and the scutellaria to find a new extraction method.

Therefore, the invention provides a honeysuckle flower and scutellaria baicalensis particle which comprises the following components in parts by weight: 60-140 parts of honeysuckle extract, 20-60 parts of scutellaria extract, 200-400 parts of medicinal dextrin and 3.0-5.0 parts of steviosin;

preferably, the Yinhuang granules comprise the following components in parts by weight: 100 parts of honeysuckle extract, 40 parts of scutellaria extract, 300 parts of medicinal dextrin and 4 parts of steviosin. The preparation method of the honeysuckle flower and scutellaria baicalensis granules comprises the following steps:

step 1, taking honeysuckle, extracting for three times by taking water as an extraction solvent, concentrating the liquid medicine, and drying to obtain a honeysuckle extract;

step 2, taking the scutellaria baicalensis, extracting twice by taking water as an extraction solvent, filtering decoction liquid, and reserving dregs for later use;

step 3, concentrating the filtrate, adding ethanol to ensure that the ethanol content in the solution is 60-80%, standing, filtering, recovering ethanol and concentrating to obtain water extract;

step 4, refluxing and extracting the dregs of a decoction twice by using ethanol, filtering an extracting solution, recovering the ethanol and concentrating to obtain an ethanol extract;

step 5, combining the water extract and the alcohol extract, and drying to obtain the scutellaria baicalensis extract;

and 6, uniformly mixing the honeysuckle extract, the scutellaria baicalensis extract, the medicinal dextrin and the steviosin, and granulating to obtain the honeysuckle-scutellaria baicalensis granules.

Preferably, the preparation method of the Yinhuang granules comprises the following steps:

step 1, extracting honeysuckle for three times by taking water as an extraction solvent, wherein the water adding amount is respectively 12 times, 8 times and 7 times, the concentration temperature is 40-70 ℃, the vacuum degree is 0.04-0.08, the concentration time is 8-10 hours, the drying temperature is 70-80 ℃, the vacuum degree is 0.06-0.08, and the drying time is 15-16 hours, so that the honeysuckle extract is obtained;

step 2, extracting the scutellaria baicalensis for 2 times by taking water as an extraction solvent, wherein the amount of water added for each time is 10 times and 6 times, decocting for 2 hours each time, filtering decoction, and reserving dregs for later use;

step 3, merging the filtrates, concentrating until the relative density is 1.05, adding 95% ethanol to ensure that the ethanol content in the solution is 70%, standing for 12 hours, filtering to obtain a supernatant, recovering the ethanol, and concentrating until a water extract with the relative density of 1.25 is obtained;

step 4, reflux-extracting the dregs of a decoction for 2 times by using 95% (V/V) ethanol, wherein the water addition amount is 8 times and 6 times of that of each time, reflux-extracting for 2 hours each time, filtering the extracting solution, combining the filtrates, recovering the ethanol, and concentrating the ethanol to obtain an ethanol extract with the relative density of 1.15;

step 5, combining the water extract and the alcohol extract, drying under reduced pressure at 80-90 ℃ under a vacuum degree of 0.06-0.08 for 6-10 hours to obtain the scutellaria baicalensis extract;

and 3, uniformly mixing the honeysuckle extract, the scutellaria baicalensis extract, the medicinal dextrin and the steviosin, and granulating to obtain the honeysuckle-scutellaria baicalensis granules.

Compared with the prior art, the preparation method of the invention has the advantages that the active ingredients of the prepared Yinhuang granules are stable under the condition of high humidity, the content of chlorogenic acid in the granules is stable between 0.3 and 0.35 percent, and simultaneously, the contents of active ingredients such as baicalin, baicalein, wogonin, oroxylin A and the like are higher than the prior art, so that the curative effect is improved.

The beneficial effects of the present invention are further illustrated by experimental data below.

Experiment one, stability experiment of granules:

experimental methods

Different samples are placed in an incubator with 40 ℃ and 75% relative humidity, the content of related substances is checked in 0 day and 60 days respectively, and the checking method adopts an HPLC method.

Drug samples:

sample 1: granulated preparation of example 1 of the invention

Sample 2: the granules are prepared according to the method under the preparation item in the standard of Yinhuang granules in the Chinese pharmacopoeia 2015 edition

Sample 3: particles prepared according to the method of chinese patent cn201010234120.x example 1

The results of the experiment are shown in the following table:

TABLE 2

The experimental result shows that the granule of the invention is superior to the prior art in the content of effective components and the stability of the preparation.

The invention improves the prior art on the basis of the prior art, particularly improves the extraction method of honeysuckle and astragalus, and unexpectedly finds that the related active ingredients of the medicine are very stable in the preparation, and the extract obtained by the extraction method of the invention has improved conversion rate or yield of the active ingredients, can save medicinal materials and reduce production cost.

Detailed Description

The invention is further illustrated by the following examples.

Example 1

The preparation method of the Yinhuang granules comprises the following steps:

step 1, extracting honeysuckle for three times by taking water as an extraction solvent, wherein the water adding amount is respectively 12 times, 8 times and 7 times, the concentration temperature is 40-70 ℃, the vacuum degree is 0.04-0.08, the concentration time is 8-10 hours, the drying temperature is 70-80 ℃, the vacuum degree is 0.06-0.08, and the drying time is 15-16 hours, so that the honeysuckle extract is obtained;

step 2, extracting the scutellaria baicalensis for 2 times by taking water as an extraction solvent, wherein the amount of water added for each time is 10 times and 6 times, decocting for 2 hours each time, filtering decoction, and reserving dregs for later use;

step 3, merging the filtrates, concentrating until the relative density is 1.05, adding 95% ethanol to ensure that the ethanol content in the solution is 70%, standing for 12 hours, filtering to obtain a supernatant, recovering the ethanol, and concentrating until a water extract with the relative density of 1.25 is obtained;

step 4, reflux-extracting the dregs of a decoction for 2 times by using 95% (V/V) ethanol, wherein the water addition amount is 8 times and 6 times of that of each time, reflux-extracting for 2 hours each time, filtering the extracting solution, combining the filtrates, recovering the ethanol, and concentrating the ethanol to obtain an ethanol extract with the relative density of 1.15;

step 5, combining the water extract and the alcohol extract, drying under reduced pressure at 80-90 ℃ under a vacuum degree of 0.06-0.08 for 6-10 hours to obtain the scutellaria baicalensis extract;

and 3, adding 2.4g of honeysuckle extract (calculated by chlorogenic acid) and 24g of scutellaria extract (calculated by baicalin) into the honeysuckle extract and the scutellaria extract according to a preparation method of the Yinhuang granular preparation required by pharmacopeia, uniformly mixing the medicinal dextrin and the steviosin, and granulating to obtain the Yinhuang granules.