阅读说明：本技术 一种热压逆流提取金银花的工艺 (Process for hot-pressing countercurrent extraction of honeysuckle ) 是由 晏业行 吕海 杨双杰 易青 张培洋 马园园 李爱华 赵姗姗 苏天君 高志红 于 2019-08-23 设计创作，主要内容包括：本发明专利涉及中药提取技术领域,公开了一种热压逆流提取金银花的工艺。它以金银花为原料,水为提取液,设置多个提取罐串联进行连续多级逆流提取,提取时利用上一级提取罐制得的提取液作为下一级提取罐的提取溶剂,逐级提取后制得最终提取液,然后经过滤、浓缩、干燥制得金银花提取物。本发明采用多级连续逆流工艺提取金银花,时间短、能耗低,提取率高,易于大规模工业化生产,提取液多级复合使用,不仅有利于增大传质速率,使得物料和提取剂接触更加充分,提高提取效率,减少废渣排出量,而且大大减少了提取溶剂用量,而辅以低温加压操作,有利于降低有效成本绿原酸的破坏率,保证提取物的品质,加快浸出和排出速率,进一步提高生产效率。(The invention relates to the technical field of traditional Chinese medicine extraction, and discloses a hot-pressing countercurrent extraction process for honeysuckle. The honeysuckle flower extract is prepared by taking honeysuckle flower as a raw material and water as an extracting solution, arranging a plurality of extracting tanks to be connected in series for continuous multi-stage countercurrent extraction, extracting step by using the extracting solution prepared by the previous extracting tank as an extracting solvent of the next extracting tank to prepare a final extracting solution, and then filtering, concentrating and drying the final extracting solution. The method adopts a multistage continuous countercurrent process to extract the honeysuckle, has short time, low energy consumption and high extraction rate, is easy for large-scale industrial production, and the extracting solution is used in a multistage composite way, thereby being beneficial to increasing the mass transfer rate, leading the contact between the material and the extracting agent to be more sufficient, improving the extraction efficiency, reducing the waste residue discharge amount, greatly reducing the using amount of the extracting solvent, assisting the low-temperature pressurization operation, being beneficial to reducing the destruction rate of the chlorogenic acid with effective cost, ensuring the quality of the extract, accelerating the leaching and discharging rate and further improving the production efficiency.)

1. The utility model provides a technology of hot pressing countercurrent extraction honeysuckle, its characterized in that uses the honeysuckle as the raw materials, and water is the extract, sets up a plurality of extraction tanks and establishes ties and carry out continuous multistage countercurrent extraction, utilizes the extract that last level extraction tank made to extract the solvent that the jar was extracted as next stage during extraction, includes the following step:

(1) adding flos Lonicerae and water into a first-stage extraction tank, introducing steam and compressed air, heating, pressurizing, leaching to obtain first-stage extractive solution and residue, and discharging residue;

(2) conveying the prepared primary extracting solution to a secondary extracting tank, adding honeysuckle, repeating the operation in the step (1) for leaching to prepare a secondary extracting solution and dregs, discharging the dregs, and repeating the operation in the same way, and performing step-by-step extraction in each extracting tank to prepare a final extract;

(3) filtering the final extract, concentrating to obtain soft extract, and drying to obtain flos Lonicerae extract.

2. The process for hot-pressing countercurrent extraction of honeysuckle as claimed in claim 1, wherein: the number of the extracting tanks is 4-6, and the corresponding extracting stages are 4-6 stages.

3. The process for hot-pressing countercurrent extraction of honeysuckle as claimed in claim 1, wherein: the adding amount of water in the first-stage extraction in the step (1) is 600-1000 Kg, and the adding amount of honeysuckle is 150-200 Kg.

4. The process for hot-pressing countercurrent extraction of honeysuckle as claimed in claim 1, wherein: in the step (1), the heating temperature is 70-80 ℃, the pressurizing pressure is 0.08-0.1MP, the leaching times are 3-4 times, and the leaching time is 1-1.5 h each time.

5. The process for hot-pressing countercurrent extraction of honeysuckle as claimed in claim 1, wherein: the mass ratio of the added amount of the honeysuckle to the material liquid of the upper-level extracting solution in each-level extraction in the step (2) is 1: 3-1: 5, and the heating temperature, the pressurizing pressure, the extraction times and the extraction time of each-level extraction are all consistent with those in the step (1).

6. The process for hot-pressing countercurrent extraction of honeysuckle as claimed in claim 1, wherein: and (3) concentrating under reduced pressure in vacuum in the step (3), wherein the vacuum degree is 0.4-0.6 Mpa, the concentration temperature is 60-80 ℃, the relative density of the thick paste is 1.2-1.25, and a microwave dryer is adopted during drying.

Technical Field

The invention relates to the technical field of traditional Chinese medicine extraction, in particular to a hot-pressing countercurrent extraction process for honeysuckle.

Background

Honeysuckle is a dry flower bud of a honeysuckle plant of the Caprifoliaceae family, is one of the traditional Chinese medicinal materials commonly used in clinic, is cold in nature and sweet in taste; has effects in clearing away heat and toxic materials, and dispelling pathogenic wind and heat, and can be used for treating carbuncle, furuncle, pharyngitis, erysipelas, dysentery, wind-heat type common cold, and fever due to epidemic febrile disease. Recent pharmacological experiments and clinical application prove that the honeysuckle extract is rich in various substances which are beneficial to human health, such as volatile oil, flavone, chlorogenic acids, triterpenes, trace elements and the like, and has stronger antibacterial action and better treatment effect on various pathogenic bacteria. The chlorogenic acid as its main active component has the medicinal functions of benefiting gallbladder, resisting bacteria, diminishing inflammation, resisting virus, stopping bleeding, increasing leucocyte, shortening blood coagulation and bleeding time, exciting central nervous system, etc. and has obvious effect in raising fragrance, protecting color, preserving freshness, etc. of food and fruit. At present, the extraction process of honeysuckle mainly comprises a water extraction method, an ethanol reflux method, a microwave method, an enzymolysis method and the like, wherein the water extraction method is simple to operate, but the extraction rate is low, and the honeysuckle needs to be boiled by adding water during extraction, the chlorogenic acid is unstable and easy to decompose in a solution at 100 ℃, so that the loss of the chlorogenic acid serving as an effective component is invisibly increased, the ethanol reflux method is large in ethanol solvent consumption, high in energy consumption and easy to leave harmful substances, and the microwave method and the enzymolysis method have a certain extraction effect, but are high in cost and high in equipment requirement, so that the large-scale industrial production requirement is difficult to meet.

Disclosure of Invention

Aiming at the problems in the prior art, the invention aims to provide a hot-pressing countercurrent extraction process for honeysuckle, which is low in energy consumption, high in extraction rate, stable and continuous, and easy to apply in a large scale.

In order to achieve the purpose, the technical scheme of the invention is as follows:

a hot-pressing countercurrent extraction process for honeysuckle flower uses honeysuckle flower as raw material, water as extracting solution, a plurality of extracting tanks are arranged in series for continuous multistage countercurrent extraction, and the extracting solution prepared by the previous extracting tank is used as the extracting solvent of the next extracting tank during extraction, and comprises the following steps:

(1) adding flos Lonicerae and water into a first-stage extraction tank, introducing steam and compressed air, heating, pressurizing, leaching to obtain first-stage extractive solution and residue, and discharging residue;

(2) conveying the prepared primary extracting solution to a secondary extracting tank, adding honeysuckle, repeating the operation in the step (1) for leaching to prepare a secondary extracting solution and dregs, discharging the dregs, and repeating the operation in the same way, and performing step-by-step extraction in each extracting tank to prepare a final extract;

(3) filtering the final extract, concentrating to obtain soft extract, and drying to obtain flos Lonicerae extract.

Preferably, the number of the extraction tanks is 4-6, and the corresponding extraction stages are 4-6 stages.

Specifically, the addition amount of water in the first-stage extraction in the step (1) is 600-1000 Kg, specifically 600Kg, 700Kg, 800Kg, 900Kg or 1000 Kg; the addition amount of the honeysuckle is 150-200 Kg, and specifically can be 150Kg, 160Kg, 170Kg, 180Kg, 190Kg or 200 Kg; the heating temperature is 70-80 ℃, and specifically 70 ℃, 72 ℃, 74 ℃, 76 ℃, 78 ℃ or 80 ℃; the pressurizing pressure is 0.08-0.1MP, the leaching times are 3-4 times, and the leaching time is 1-1.5 h each time.

Specifically, the mass ratio of the added amount of the honeysuckle to the feed liquid of the upper-level extracting solution in each-level extraction in the step (2) is 1: 3-1: 5, and the heating temperature, the pressurizing pressure, the extraction frequency and the extraction time in each-level extraction are all consistent with those in the step (1).

Specifically, vacuum reduced pressure concentration is adopted during concentration in the step (3), the vacuum degree is 0.4-0.6 Mpa, and the concentration temperature is 60-80 ℃, specifically 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃; the relative density of the thick paste is 1.2-1.25, and a microwave dryer is adopted for drying during drying.

Compared with the prior art, the invention has the advantages that:

1. the hot-pressing countercurrent extraction process for honeysuckle provided by the invention has the advantages of low energy consumption, high extraction rate, stability and continuity, and is easy for large-scale industrial production.

2. The method adopts a multistage continuous countercurrent process to extract the honeysuckle, the extracting solution prepared by the previous stage extracting tank is used as the extracting solvent of the next stage extracting tank during extraction, and after the extraction step by step, the concentration of the extract is gradually increased, so that the mass transfer rate is increased, the contact between the material and the extracting agent is more sufficient, the extraction efficiency is improved, the waste residue discharge amount is reduced, and the using amount of the extracting solvent is greatly reduced.

3. The process for extracting the honeysuckle by hot-pressing countercurrent provided by the invention is assisted with low-temperature pressurization operation during extraction, so that the destruction rate of chlorogenic acid with effective cost is greatly reduced, the quality of the honeysuckle extract is ensured, meanwhile, the proper heating temperature is more favorable for the leaching speed of effective components, and the production efficiency is improved; the pressure is increased, so that the solvent can quickly permeate the medicinal materials, the dissolution and balance of the components in the medicinal materials are accelerated, and meanwhile, the proper external pressure can accelerate the filtering speed of the extracting solution during liquid drainage.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the 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.

Example 1

A hot-pressing countercurrent extraction process for honeysuckle flower uses honeysuckle flower as raw material, water as extracting solution, 4 extracting tanks are arranged in series for continuous 4-stage countercurrent extraction, and the extracting solution prepared by the previous extracting tank is used as the extracting solvent of the next extracting tank during extraction, and comprises the following steps:

(1) adding 150Kg of honeysuckle and 600Kg of water into a first-stage extraction tank from a feed inlet, opening a steam valve, heating an interlayer of the extraction tank, keeping the temperature in the tank at 70 ℃, simultaneously introducing compressed air into the first-stage extraction tank, pressurizing until the pressure in the tank reaches 0.08Mp, continuously extracting for 4 times, wherein the extraction time is 1h each time, preparing a first-stage extracting solution and dregs, and discharging the dregs;

(2) conveying the prepared primary extracting solution to a secondary extracting tank, adding honeysuckle according to the material liquid mass ratio of 1:3, repeating the operation in the step (1) for leaching to prepare a secondary extracting solution and dregs, discharging the dregs, and repeating the steps in the same manner, and performing 4-stage extraction to obtain a final extract;

(3) filtering the final extract, concentrating the filtrate under 0.4Mpa under reduced pressure to 80 deg.C to obtain soft extract with relative density of 1.2, and drying in microwave dryer to obtain flos Lonicerae extract.

(4) The detection results of the above honeysuckle extract, the yield of chlorogenic acid and the extraction rate of chlorogenic acid are shown in table 1.

Example 2

A hot-pressing countercurrent extraction process for honeysuckle flower uses honeysuckle flower as raw material, water as extracting solution, 5 extracting tanks are arranged in series for continuous 5-stage countercurrent extraction, and the extracting solution prepared by the previous extracting tank is used as an extracting solvent of the next extracting tank during extraction, and comprises the following steps:

(1) adding 170Kg of honeysuckle and 800Kg of water into a first-stage extraction tank from a feed inlet, opening a steam valve, heating an interlayer of the extraction tank, keeping the temperature in the tank at 76 ℃, simultaneously introducing compressed air into the first-stage extraction tank, pressurizing until the pressure in the tank reaches 0.09Mp, continuously leaching for 3 times, wherein the leaching time is 1.5h each time, preparing first-stage extracting solution and dregs, and discharging the dregs;

(2) conveying the prepared primary extracting solution to a secondary extracting tank, adding honeysuckle according to the material liquid mass ratio of 1:4, repeating the operation in the step (1) for leaching to prepare a secondary extracting solution and dregs, discharging the dregs, and repeating the steps in the same manner, and performing 5-stage extraction to obtain a final extract;

(3) filtering the final extract, concentrating the filtrate under 0.5Mpa under reduced pressure to 70 deg.C to obtain soft extract with relative density of 1.22, and drying in microwave dryer to obtain flos Lonicerae extract.

(4) The detection results of the above honeysuckle extract, the yield of chlorogenic acid and the extraction rate of chlorogenic acid are shown in table 1.

Example 3

A hot-pressing countercurrent extraction process for honeysuckle flower uses honeysuckle flower as raw material, water as extracting solution, 6 extracting tanks are arranged in series for continuous 6-stage countercurrent extraction, and the extracting solution prepared by the previous extracting tank is used as an extracting solvent of the next extracting tank during extraction, and comprises the following steps:

(1) adding 200Kg of honeysuckle and 1000Kg of water into a first-stage extraction tank from a feed inlet, opening a steam valve, heating an interlayer of the extraction tank, keeping the temperature in the tank at 80 ℃, simultaneously introducing compressed air into the first-stage extraction tank, pressurizing until the pressure in the tank reaches 0.1Mp, continuously extracting for 4 times, wherein the extraction time is 1.2h each time, preparing a first-stage extracting solution and dregs, and discharging the dregs;

(2) conveying the prepared primary extracting solution to a secondary extracting tank, adding honeysuckle according to the material liquid mass ratio of 1:5, repeating the operation in the step (1) for leaching to prepare a secondary extracting solution and dregs, discharging the dregs, and repeating the steps in the same manner, and performing 6-stage extraction to obtain a final extract;

(3) filtering the final extract, concentrating the filtrate under 0.6Mpa under reduced pressure to 60 deg.C to obtain soft extract with relative density of 1.25, and drying in microwave dryer to obtain flos Lonicerae extract.

(4) The detection results of the above honeysuckle extract, the yield of chlorogenic acid and the extraction rate of chlorogenic acid are shown in table 1.

Comparative example

A preparation process of a honeysuckle extract comprises the following steps:

(1) selecting dried honeysuckle, removing impurities, and cutting into strips of 1-3 cm;

(2) the material-liquid ratio is 1: 3-1: 5, respectively adding the strip-shaped honeysuckle and the extraction solvent into an extraction tank for reflux extraction, wherein the reflux extraction temperature is 55-95 ℃, the extraction times are 4-6 times, and the extraction time is 0.5-2 hours each time, filtering the extract after the extraction is finished, and combining the filtrates;

(3) and concentrating the obtained filtrate under reduced pressure to obtain thick paste with the relative density of 1.2-1.25, and drying the thick paste to obtain the honeysuckle extract.

(4) The detection results of the above honeysuckle extract, the yield of chlorogenic acid and the extraction rate of chlorogenic acid are shown in table 1.

Table 1 shows the cream yield, chlorogenic acid yield and chlorogenic acid extraction rate of the honeysuckle extracts prepared in examples 1-3 and comparative examples of the present invention.

Item	Percentage of cream discharged (%)	Chlorogenic acid yield (%)	Chlorogenic acid extraction ratio (%)
				Example 1	38.54	80.19	86.23
Example 2	40.36	83.52	88.16
				Example 3	39.21	81.64	84.55
Comparative example	33.89	70.21	76.39

The determination method of the extract in table 1 is carried out according to each method under the item of honeysuckle in the version 2010 of the Chinese pharmacopoeia, and the chromatographic conditions are as follows: c18 column, acetonitrile-0.4% phosphoric acid solution (13: 78) as mobile phase, detection wavelength 327 nm.

As can be seen from Table 1, compared with the conventional extraction process, the hot-pressing countercurrent extraction process for honeysuckle provided by the invention has the advantages that the cream yield, the chlorogenic acid yield, the extraction rate and the content are obviously improved, and the effect of the example 2 is better.

The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.