阅读说明：本技术 一种稳定性较高的柴胡注射液及其制备方法 (Radix bupleuri injection with high stability and preparation method thereof ) 是由 雷变兰 马泽宁 柴清珍 朱增民 朱翀 白小军 于 2020-08-29 设计创作，主要内容包括：本发明提供的一种稳定性较高的柴胡注射液,包括：以下重量份的原料：柴胡药材800~1500份、20~50份乙醇、泊洛沙姆2~4份、吐温-80 2~4份、氯化钠3~15份、盐酸3~15份和注射用水600~1500份；其制备方法包括以下步骤：称取原料；粉碎柴胡药材；向柴胡粉末中加入300~500份蒸馏水,搅拌均匀,将温度提升至60~80℃,保温10~20min；蒸馏；浓缩；醇沉；然后在上清液中加入泊洛沙姆、吐温-80和氯化钠,搅拌溶解,在40~50℃下浸渍1.5~2.5h；过滤,得到滤液和滤饼；向滤液中加入盐酸、注射用水,将pH值调节至4.0~7.0；精滤、灌封、灭菌即可；本发明具有稳定性较高的有益效果,适用于制药领域。(The invention provides a bupleurum injection with higher stability, which comprises the following components: the following raw materials in parts by weight: 800-1500 parts of radix bupleuri medicinal material, 20-50 parts of ethanol, 2-4 parts of poloxamer, 802-4 parts of tween-4, 3-15 parts of sodium chloride, 3-15 parts of hydrochloric acid and 600-1500 parts of water for injection; the preparation method comprises the following steps: weighing raw materials; pulverizing bupleuri radix; adding 300-500 parts of distilled water into the radix bupleuri powder, uniformly stirring, raising the temperature to 60-80 ℃, and preserving the heat for 10-20 min; distilling; concentrating; precipitating with ethanol; then adding poloxamer, tween-80 and sodium chloride into the supernatant, stirring to dissolve, and soaking for 1.5-2.5 h at 40-50 ℃; filtering to obtain filtrate and filter cake; adding hydrochloric acid and water for injection into the filtrate, and adjusting the pH value to 4.0-7.0; fine filtering, bottling, and sterilizing; the invention has the beneficial effect of higher stability and is suitable for the pharmaceutical field.)

1. A bupleurum injection with higher stability is characterized in that: the feed comprises the following raw materials in parts by weight: 800-1500 parts of radix bupleuri, 20-50 parts of ethanol, 2-4 parts of poloxamer, 802-4 parts of tween-802, 3-15 parts of sodium chloride, 3-15 parts of hydrochloric acid and 600-1500 parts of water for injection.

2. The bupleurum injection with higher stability as claimed in claim 1, wherein: the concentration of the hydrochloric acid is 0.1-0.3%.

3. The bupleurum injection with higher stability as claimed in claim 1, wherein: the concentration of the sodium chloride is 15-25%.

4. A method for preparing bupleuri radix injection with high stability as claimed in any one of claims 1-3, wherein the method comprises: the method comprises the following steps:

(1) weighing the following raw materials: bupleurum medicinal material, poloxamer, tween-80, sodium chloride, hydrochloric acid and water for injection;

(2) crushing: pulverizing bupleuri radix into powder;

(3) adding 300-500 parts of distilled water into the radix bupleuri powder, uniformly stirring, raising the temperature to 60-80 ℃, and preserving the heat for 10-20 min;

(4) and (3) distillation: extracting by steam distillation, collecting primary distillate, redistilling the primary distillate, and collecting redistillate;

(5) concentration: concentrating the obtained redistillate, condensing steam generated by concentration, adding the steam as a new solvent again, continuously repeating the step during extraction, wherein the extraction time is 0.5-2 h, and obtaining the bupleurum volatile oil after the extraction is finished;

(6) alcohol precipitation: adding 95% ethanol into bupleuri radix volatile oil, precipitating with ethanol until the ethanol concentration is 70%, standing for 12 hr, and collecting supernatant after ethanol precipitation;

(7) then adding poloxamer, tween-80 and sodium chloride into the supernatant, stirring to dissolve, and soaking for 1.5-2.5 h at 40-50 ℃; filtering to obtain filtrate and filter cake;

(8) adding hydrochloric acid and water for injection into the filtrate, and adjusting the pH value to 4.0-7.0; fine filtering, bottling, and sterilizing.

5. The preparation method of the bupleurum injection with higher stability as claimed in claim 4, wherein: the concentration is reduced pressure concentration, the temperature of the reduced pressure concentration is 50-70 ℃, and the pressure is 0.08-0.09 Mpa.

6. The preparation method of the bupleurum injection with higher stability as claimed in claim 4, wherein: the particle size of the bupleurum powder in the step 2 is 30-50 meshes.

7. The preparation method of the bupleurum injection with higher stability as claimed in claim 4, wherein: the water consumption of the steam distillation in the step 4 is the same as the addition of the bupleurum medicinal material.

8. The preparation method of the bupleurum injection with higher stability as claimed in claim 4, wherein: introducing N into the can before filling and sealing₂Or CO₂Gas and then encapsulated.

Technical Field

The invention relates to the technical field of pharmacy, in particular to a bupleurum injection with higher stability and a preparation method thereof.

Background

The bupleurum is a traditional Chinese medicine and a commonly used Chinese medicine in China and is a herbal medicine recorded in Chinese pharmacopoeia, and the medicinal part of bupleurum, namely bupleurum medicinal material, is the dried root of bupleurum or bupleurum stenophyllum of umbelliferae. Collected in spring and autumn, removed stems and leaves and silt, and dried. Bupleurum root, radix bupleuri is a commonly used exterior syndrome relieving drug. Is also called as Diwu, potherb mustard, mushroom grass and firewood, is bitter in nature and taste, slightly cold, and enters liver and gallbladder meridians. Has the functions of harmonizing exterior and interior, soothing liver and invigorating yang. Can be used for treating common cold, fever, malaria, stagnation of qi due to depression of the liver, distending pain of chest and hypochondrium, rectocele, uterine prolapse, and menoxenia, and has high medicinal value.

The bupleurum injection prepared from bupleurum medicinal materials is used for treating fever such as cold, influenza, malaria and the like. However, the stability of the bupleurum injection is difficult to guarantee, the PH value of the injection can obviously float after being stored for a certain time, and the storage time is short. Therefore, the stability of the bupleurum injection is improved, which has important significance.

Disclosure of Invention

Aiming at the defects in the related technology, the technical problem to be solved by the invention is as follows: provides a bupleurum injection with higher stability and a preparation method thereof.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a bupleurum injection with higher stability comprises the following raw materials in parts by weight: 800-1500 parts of radix bupleuri, 20-50 parts of ethanol, 2-4 parts of poloxamer, 802-4 parts of tween-802, 3-15 parts of sodium chloride, 3-15 parts of hydrochloric acid and 600-1500 parts of water for injection.

Preferably, the concentration of the hydrochloric acid is 0.1-0.3%.

Preferably, the concentration of the sodium chloride is 15-25%.

The invention also provides a preparation method of the bupleurum injection with higher stability as recited in any one of claims 1 to 3, which comprises the following steps: (1) weighing the following raw materials: bupleurum medicinal material, poloxamer, tween-80, sodium chloride, hydrochloric acid and water for injection; (2) crushing: pulverizing bupleuri radix into powder; (3) adding 300-500 parts of distilled water into the radix bupleuri powder, uniformly stirring, raising the temperature to 60-80 ℃, and preserving the heat for 10-20 min; (4) and (3) distillation: extracting by steam distillation, collecting primary distillate, redistilling the primary distillate, and collecting redistillate; (5) concentration: concentrating the obtained redistillate, condensing steam generated by concentration, adding the steam as a new solvent again, continuously repeating the step during extraction, wherein the extraction time is 0.5-2 h, and obtaining the bupleurum volatile oil after the extraction is finished; (6) alcohol precipitation: adding 95% ethanol into bupleuri radix volatile oil, precipitating with ethanol until the ethanol concentration is 70%, standing for 12 hr, and collecting supernatant after ethanol precipitation; (7) then adding poloxamer, tween-80 and sodium chloride into the supernatant, stirring to dissolve, and soaking for 1.5-2.5 h at 40-50 ℃; filtering to obtain filtrate and filter cake; (8) adding hydrochloric acid and water for injection into the filtrate to adjust the pH value to 4.0-7.0; fine filtering, bottling, and sterilizing.

Preferably, the temperature of the reduced pressure concentration is 50-70 ℃, and the pressure is 0.08-0.09 Mpa.

Preferably, the particle size of the bupleurum powder in the step 2 is 30-50 meshes.

Preferably, the amount of water used for steam distillation in step 4 is the same as the amount of bupleurum root.

Preferably, N is introduced into the can before filling and sealing₂Or CO₂Gas and then encapsulated.

The specification of the prepared bupleurum injection is 10 ml: 10 g.

The using method comprises the following steps: intramuscular or intravenous injection, 20-40 ml of horse and cattle; 5-10 ml of sheep and pigs.

The invention has the beneficial technical effects that:

1. the bupleurum injection provided by the invention comprises ethanol and poloxamer, the ethanol is used for carrying out alcohol precipitation on the bupleurum volatile oil, the poloxamer is added, the solubility of the bupleurum injection can be further improved, the use of a solubilizer Tween-80 is reduced, and the prepared bupleurum injection has higher stability.

The bupleurum medicinal material, ethanol, poloxamer, tween-80, sodium chloride, hydrochloric acid and water for injection are reasonably compatible, and the prepared bupleurum injection has higher stability under the combined action of the raw materials.

2. The method has the advantages that the bupleurum medicinal material is crushed, distilled and concentrated, so that the medicinal components in the bupleurum medicinal material can be effectively extracted into the bupleurum volatile oil, and the yield is high; continuously concentrating and extracting for 0.5-2 h in the concentration process, and fully extracting medicinal components of the radix bupleuri in the redistillate; precipitating bupleuri radix volatile oil with ethanol to obtain supernatant with high purity; adding poloxamer, tween-80 and sodium chloride into the supernatant, stirring for dissolving, soaking for 1.5-2.5 h at 40-50 ℃, fully dissolving the supernatant, the poloxamer, the tween-80 and the sodium chloride together through soaking, and filtering to obtain a filtrate with stable solvent and difficult precipitation; then adding hydrochloric acid and water for injection, adjusting the pH value to 4.0-7.0, and after the pH value is adjusted, the prepared bupleurum injection is more stable and can be stored for a longer time at normal temperature.

3. The concentration is reduced pressure concentration, the temperature of the reduced pressure concentration is 50-70 ℃, and the pressure is 0.06-0.09 Mpa. According to the invention, the heavy distillate is subjected to reduced pressure concentration in a reduced pressure concentration mode, the reduced pressure concentration effect is best under the conditions that the temperature is 50-70 ℃ and the pressure is 0.06-0.09 Mpa, and the bupleurum volatile oil in the heavy distillate can be completely extracted.

4. The bupleurum medicinal material is crushed into bupleurum powder with the particle size of 30-50 meshes, so that the medicinal components in the bupleurum can be more effectively extracted, and the filtration is convenient.

5. N is introduced into the can before filling and sealing₂Or CO₂Gas and then encapsulated. Introduction of N₂Or CO₂The gas can discharge oxygen in the bottle to prevent the prepared bupleuri radix injection from being oxidized.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments, and it is obvious that the described embodiments are some embodiments, but not all embodiments, of the present invention; all other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

In the actual process of preparing the bupleurum injection with higher stability, the weight parts of the raw materials correspond to the grams.

In particular, 1 part of a proportion equal to 1g is used in the preparation.