CN102391116B

CN102391116B - Method for extracting chlorogenic acid from honeysuckle flower leaves

Info

Publication number: CN102391116B
Application number: CN201110292698.5A
Authority: CN
Inventors: 祝利; 赵勇彪; 杨再江; 向延军; 何全慧
Original assignee: CHONGQING XIUSHAN RED STAR TCM DEVELOPMENT Co Ltd
Current assignee: CHONGQING XIUSHAN RED STAR TCM DEVELOPMENT Co Ltd
Priority date: 2011-10-05
Filing date: 2011-10-05
Publication date: 2014-03-05
Anticipated expiration: 2031-10-05
Also published as: CN102391116A

Abstract

The invention relates to a method for extracting chlorogenic acid from honeysuckle flower leaves. The method comprises the following steps of: crushing, soaking, filtering, eluting, concentrating, drying, packaging in separate bags and the like. By the method, effective resources are utilized to a maximum limit, economic benefit is increased, food grade ethanol is used as an extractant and a purifying agent in the production process, and the chlorogenic acid is extracted at normal temperature, so the production cost is reduced, and the chlorogenic acid is prevented from being decomposed; the honeysuckle flower leaves are soaked for multiple times in the soaking process, and extraction solution is obtained, so the purity is improved effectively; and purification and elution are performed by using macroporous resin, so that the purity of the chlorogenic acid is improved greatly to 35 to 95 percent according to requirements.

Description

The method of chlorogenic acid extracting from leaf of Flos Lonicerae

Technical field

The present invention relates to a kind of method of chlorogenic acid extracting, particularly a kind of from leaf of Flos Lonicerae the method for chlorogenic acid extracting.

Background technology

Japanese Honeysuckle belongs to caprifoliaceae plant, and herb all can be used as medicine, and bud contains volatile aromatic oil, inositol, saponin(e, chlorogenic acid, flavonoid compound, styracin, vernol, α-amyl cinnamic aldehyde etc., in stem, containing alkaloid, contain lonicerin and sweet-scented osmanthus element etc. in leaf, is one of traditional Chinese medicine material, also be the raw material of medicine-food two-purpose, have clearing heat and detoxicating, wind-heat dissipating, the effect of hepatic cholagogic, in traditional Chinese medical science field always for the swollen furunculosis of carbuncle, larynx numbness, erysipelas, toxic-heat and blood stasis, common cold due to wind-heat, the treatment of warm morbidity; Particularly in gold and silver bud, stem, leaf, all contain chlorogenic acid, chlorogenic acid has good effect to preventing and treating upper respiratory tract infection, common cold due to wind-heat and gastroenteropathy, to removing human free radical, delay senility, improve human immunologic function etc. and have good effect; Thereby chlorogenic acid extracting is the important topic of pharmacy field, traditional chlorogenic acid extraction process is chlorogenic acid extracting from Japanese Honeysuckle only mostly, has ignored the extraction of cauline leaf Content of Chlorogenic Acid, serious waste efficient resource.

Summary of the invention

Technical problem to be solved by this invention is to provide a kind of method of utilizing leaf of Flos Lonicerae chlorogenic acid extracting, to obtain to greatest extent efficient resource, cuts the waste.

For solving the problems of the technologies described above, the technical solution adopted in the present invention by pulverizing, soak, filtration, wash-out, concentrated, dry, packing form, specific as follows.

(1) pulverize: leaf of Flos Lonicerae is cleaned, is dried, is pulverized, and size of powder particles is 20～40 orders.

(2) soak: minute soak and extract filtrate three times, merging filtrate then, operation steps is as follows:

For the first time: powder is immersed in ethanolic soln, and alcohol concn is 65～75%, and solid-to-liquid ratio is 1kg:8～10L, soak time 45～55min, filters and obtains extracting solution, leaves filter residue;

For the second time: filter residue being added to concentration is 65～75% ethanol 10～12L, soaks 35～45min again, filter and obtain extracting solution, leave filter residue;

For the third time: will be for the second time filter residue to add concentration be 65～75% ethanol 8～10L, soak 30-40min, filter and obtain extracting solution; Then the extracting solution that merges three times is stand-by.

(3) filter: in extracting solution, add finings, fully stir latter standing 10～14 hours, the albumen in precipitation solution, tannin, natural gum and impurity, separation of supernatant and throw out, then filter and obtain supernatant liquor filtrate.

(4) wash-out: with macroporous resin adsorption supernatant liquor filtrate, flow rate control is at 400～600L/hr; Then use purified water wash-out, flow rate control is 300～500L/hr, and the overall control of purified water elutriant is about 0.5～1 times of resinite accumulated amount, discards elutriant; With the ethanolic soln wash-out that pH value is 2～3, concentration is 45～65%, flow rate control is at 400～600L/hr again, and elutriant (50% ethanol) overall control is about 3 times of resinite accumulated amounts, finally reclaims the elutriant that contains chlorogenic acid.

(5) concentrated: it is 1.15～1.20(50 ℃ of survey that the elutriant that contains chlorogenic acid is concentrated into relative density by nanofiltration) concentrated solution.

(6) dry: by vacuum, to suck through the concentrated concentrated solution of nanofiltration thickening equipment, vacuum tightness is that 0.01～0.08Mpa, drying temperature are controlled at 60 ℃ following (keep water tank temperature at 85～95 ℃, charging stock tank temperature is controlled at 45～65 ℃), input speed 180～200mm/min; And receive powder and pack middle turning barrel into, weigh and stick bucket and sign, be placed in material temporary between, censorship intermediates.

(7) packing: treat that this product is up to the standards after (moisture≤8.0%, bacterium must not be more than 800/g, must not be more than 80/g containing mould, escherichia coli must not detect), clean rank be between the clean packaging of 100,000 grades in packing; Proceeding to shady and cool storehouse (18～26 ℃ of temperature, relative humidity 45～75%) preserves.

The present invention has utilized efficient resource to greatest extent, increased economic benefit, used in process of production food grade ethanol as extraction agent and purifying agent, and extracted at normal temperatures, can reduce production costs, avoid chlorogenic acid to decompose, in immersion process, repeatedly soak and get liquid, effectively improved purity, then with macroporous resin, purify and wash-out, greatly improved the purity of chlorogenic acid, as required, can make the 35-95% that reaches of chlorogenic acid purity.

Accompanying drawing explanation

Accompanying drawing is the process flow sheet of the present invention's method of chlorogenic acid extracting from leaf of Flos Lonicerae.

Embodiment

Below in conjunction with embodiment, the invention will be further described.

Dry leaf of Flos Lonicerae 10kg after roughing is pulverized, cross sieve No. four; Then powder is immersed in 100L ethanolic soln, alcohol concn is 70%, and soak time 50min filters and obtains extracting solution, leaves filter residue; Then filter residue being added to concentration is 70% ethanol 110L, soaks 40min, filters and obtains extracting solution, leaves filter residue; Then for the second time filter residue to add concentration be 70% ethanol 90L, soak 35min, filter and obtain extracting solution; Then the extracting solution that merges three times is stand-by.

In extracting solution, add finings, fully stir latter standing 12 hours, separation of supernatant and throw out, then filter and obtain supernatant liquor filtrate; The macroporous resin that is 0.8mm with particle diameter again adsorbs supernatant liquor filtrate by supernatant liquor, and flow velocity is 500L/hr; Then use purified water wash-out, flow velocity is 400L/hr, and purified water elutriant total amount is 1 times of resinite accumulated amount, discards elutriant; With the ethanolic soln wash-out that pH value is 2.5, concentration is 55%, flow velocity is 500L/hr again, and elutriant (50% ethanol) is 3 times of resinite accumulated amounts, finally reclaims the elutriant that contains chlorogenic acid.

It is 1.15(50 ℃ of survey that the elutriant that contains chlorogenic acid is concentrated into relative density by nanofiltration) concentrated solution, then by vacuum, suck through the concentrated concentrated solution of nanofiltration thickening equipment, vacuum tightness is that 0.05Mpa, drying temperature control are 55 ℃ (keeping water tank temperature is 90 ℃, and it is 60 ℃ that charging stock tank temperature is controlled), input speed 190mm/min; And receive powder and pack middle turning barrel into, weigh and stick bucket and sign, be placed in material temporary between, then censorship intermediates.

(moisture≤8.0% will be up to the standards, bacterium must not be more than 800/g, must not be more than 80/g containing mould, escherichia coli must not detect) product be placed on clean rank be between the clean packaging of 100,000 grades in packing, then proceed to shady and cool storehouse (18～26 ℃ of temperature, relative humidity 45～75%) and preserve.

Claims

1. the method for chlorogenic acid extracting from leaf of Flos Lonicerae, is comprised of pulverizing, immersion, filtration, wash-out, concentrated, dry and packing step, it is characterized in that concrete steps are as follows:

(1) pulverize: leaf of Flos Lonicerae is cleaned, is dried, is pulverized, cross sieve No. four;

(2) soak: divide and soak and extract filtrate, then merging filtrate three times;

(3) filter: in extracting solution, add finings, fully stir latter standing 10～14 hours, the albumen in precipitation solution, tannin, natural gum and impurity, separation of supernatant and throw out, then filter and obtain supernatant liquor filtrate;

(4) wash-out: with macroporous resin adsorption supernatant liquor filtrate, flow rate control is at 400～600L/hr; Then use purified water wash-out, flow rate control is 300～500L/hr, and the overall control of purified water elutriant is 0.5～1 times of resinite accumulated amount, discards elutriant; With the ethanolic soln wash-out that pH value is 2～3, concentration is 45～65%, flow rate control is at 400～600L/hr again, and elutriant overall control is 3 times of resinite accumulated amounts, finally reclaims the elutriant that contains chlorogenic acid;

(5) concentrated: it is 1.15～1.20 concentrated solution that the elutriant that contains chlorogenic acid is concentrated into relative density by nanofiltration, and the temperature condition of this relative density test is 50 ℃;

(6) dry: by vacuum, to suck concentrated solution and be dried, obtain chlorogenic acid powder, collect chlorogenic acid powder and pack middle turning barrel into, weigh and stick bucket and sign, be placed between material keeps in censorship intermediates;

(7) packing: treat chlorogenic acid powder after the assay was approved, clean rank be between the clean packaging of 100,000 grades in packing; Finally proceed to shady and cool storehouse and preserve, wherein shady and cool warehouse temperature is that 18～26 ℃, relative humidity are 45～75%; The standard being wherein up to the standards is moisture≤8.0%, and bacterium must not be more than 800/g, and containing mould must not be more than 80/g, and escherichia coli must not detect;

Wherein step (2) described immersion refer to and minute soak and extract filtrate three times, merging filtrate then, concrete operation step is as follows:

(1) for the first time: powder is immersed in ethanolic soln, and alcohol concn is 65～75%, and solid-to-liquid ratio is 1kg:8～10L, soak time 45～55min, filters and obtains extracting solution, leaves filter residue;

(2) for the second time: filter residue being added to concentration is 65～75% ethanol 10～12L, soaks 35～45min again, filter and obtain extracting solution, leave filter residue;

(3) for the third time: will be for the second time filter residue to add concentration be 65～75% ethanol 8～10L, soak 30-40min, filter and obtain extracting solution;

(4) the extracting solution that merges three times is stand-by;

Wherein step is (6) described dryly refers to that by vacuum, sucking concentrated solution is dried, and vacuum tightness is that 0.01～0.08MPa, drying temperature are controlled at 60 ℃ of following, maintenance water tank temperatures at 85～95 ℃, charging stock tank temperature, to be controlled at 45～65 ℃, input speed be 180～200mm/min.