CN104666430B - A kind of method that jasmine general flavone is extracted in response phase method optimization - Google Patents

Abstract

The invention discloses the method that jasmine general flavone is extracted in a kind of optimization of response phase method, optimum extraction process is determined according to Box Behnken designs using design expert softwares：Solution pH 5.5~6, liquid-solid ratio 15~20: 1, raw material dipping 10~20 minutes, 85~92 DEG C of Extracting temperature, naturally 20~30 minutes ultrasonic wave extraction time, chromatography 0.5~1 hour.The solvent dimethyl carbonate that the present invention is used is a kind of to integrate spatter property and the green solvent of security, the cavitation of ultrasonic wave, second order effect make use of to accelerate the dispersal events of jasmine active component and fully be mixed with solvent, complete beneficial to extracting, product yield is up to 98.6%.This method technological process is short, and operation is easy, and extraction time is short, and solvent loss is few, energy-conserving and environment-protective, and product yield is high, and product cost is low, the danger in production is greatly reduced, with preferable economic benefit, social benefit and ecological benefits.

Description

A method for optimal extraction of total flavonoids from jasmine by response surface methodology

technical field

The invention relates to a method for extracting plants, in particular to a method for optimally extracting jasmine total flavonoids by response surface method, and belongs to the technical field of traditional Chinese medicines.

Background technique

The incidence of cardiovascular disease is increasing year by year in all countries in the world, and it has become the "number one killer" that threatens human health beyond cancer, and is the main cause of death of patients. According to WHO's statistics on the death of various diseases in the world, the number of deaths due to cardiovascular and cerebrovascular diseases accounts for about 30% of the total number of deaths, causing huge spiritual and economic burdens to the people and society. At present, the clinical treatment of ischemic heart disease such as hypertension and coronary heart disease is still based on drugs, including commonly used β receptor blockers, calcium antagonists, angiotensin converting enzyme inhibitors, angiotensin Western medicines such as II receptor antagonists, as well as traditional Chinese medicine preparations with definite curative effects such as ginkgo biloba and chrysanthemum. However, due to the protection of intellectual property rights, the high price of imported drugs, and the tolerance and side effects that may occur when taking western medicines, it is of great social significance to promote the development of traditional Chinese medicine to benefit the country and the people by discovering the treasures of traditional Chinese medicine and developing drugs with self-owned intellectual property rights.

Jasminum samba (Jasminum samba) is an angiosperm, Oleaceae, Jasminum (or Jasmine) plant, native to India, and now it is widely cultivated in Guangxi, Guangdong, Jiangsu, Sichuan, Fujian, Yunnan and other places in my country, and has become the world's largest jasmine flower. The country with the largest production. The national jasmine cultivation area has reached 3333 hm ² , accounting for about 2/3 of the world's cultivation area, and the annual output accounts for more than 50% of the world's total jasmine production. Jasmine has a very long flowering period, from May in early summer to October in late autumn, and the flowers bloom in an endless stream. Its roots, stems, leaves and flowers are all treasures and have medicinal value. According to "Compendium of Materia Medica", jasmine, pungent, sweet, cool, regulating qi, and neutralizing, can be decocted to treat diarrhea and abdominal pain, decocted and washed with water to treat conjunctivitis; Stir-fry the rotten wine and pack it on the affected area to treat bruises, muscle and bone pain, grind boiled egg yolk and mix it thoroughly, stuff it into caries holes to treat dental caries, and take it with ground water to treat insomnia.

The extraction methods of total flavonoids of jasmine are conventional petroleum ether extraction, alcohol extraction, water extraction and CO ₂ supercritical extraction. The existing extraction method has complex technological process, difficult operation, long time, high energy consumption, low yield, large solvent loss, environmental pollution and high product cost.

Dimethyl carbonate (Dimethyl carbonate, abbreviated DMC) is a colorless, transparent liquid with an aromatic odor. It has a wide range of sources. It can be synthesized not only by petrochemical and coal chemical routes, but also by renewable resources. In addition, it can be synthesized by greenhouse Gas _CO2 is used to synthesize dimethyl carbonate, which not only solves environmental problems, but also utilizes cheap carbon sources. Dimethyl carbonate has the characteristics of non-toxic, non-corrosive, high oxygen content, narrow range of melting point and boiling point, high surface tension, low viscosity, small dielectric constant and good compatibility. Its molecular structure contains methyl, carbonyl and formazan It has three functional groups of ester group and excellent solubility. It is known as the cornerstone of green chemical raw materials and green chemical products in the 21st century. It is an environmentally friendly chemical raw material that meets the requirements of modern clean technology. In 1992, DMC passed the Nontoxic substance) registration. Dimethyl carbonate contains methyl, methoxy and carbonyl groups, which can replace highly toxic phosgene as a carbonylating agent, and can also replace carcinogenic dimethyl sulfate as a methylating agent; dimethyl carbonate can replace chlorine Fluorocarbons, trichloroethane and other substances that destroy the ozone layer of the atmosphere are used as cleaning agents and can also be used in the pharmaceutical industry; in the paint, coating and adhesive industries, dimethyl carbonate can replace toluene-based toxic solvents.

Contents of the invention

The purpose of the present invention is to provide a method for optimizing the extraction of total flavonoids of jasmine by using response surface methodology, optimizing the factors affecting the extraction of total flavonoids of jasmine such as extraction pH value, extraction temperature, extraction time and liquid-solid ratio, thereby improving the extraction of total flavonoids of jasmine Improve the yield, shorten the extraction time, reduce energy consumption and product cost, improve the quality and resource utilization of jasmine total flavonoids, and promote drug safety.

Technical scheme of the present invention is:

A method for optimizing the extraction of total flavonoids of jasmine by response surface methodology, using design expert software to design and extract the solvent pH value, temperature, time and liquid-solid ratio process conditions of jasmine as raw material according to Box-Behnken, using ultrasonic Auxiliary extraction of jasmine total flavonoids, including the following process steps:

(1) Raw material crushing: crush the jasmine flowers, stems and leaves respectively, and set aside;

(2) Impregnation: Put the broken jasmine flowers, stems or leaves into the extraction tank, add solvent at a liquid-solid ratio of 15-20:1, and impregnate for 10-20 minutes;

(3) Extraction: After dipping, heat up to 85-92°C, start ultrasonic, control the time for 20-30 minutes, filter, extract 2-3 times, and combine the filtrates;

(4) Separation: Place the combined filtrate of step (3) in a natural chromatography tank for natural chromatography for 0.5 to 1 hour, discharge the solvent and continue to use it for the next batch of production solvents;

(5) Purification: Add the extract of total flavonoids of jasmine separated in step (4) into a purification tank, continue natural chromatography, filter, or use vacuum distillation to obtain total flavonoids of jasmine.

The solvent mentioned above is dimethyl carbonate, and the pH value of the solvent is adjusted to 5.5-6 with hydrochloric acid, acetic acid or sodium hydroxide.

The ultrasonic control frequency mentioned above is 40-50 kHz.

The crushing mentioned above selects extruder, crusher or roller press.

The above-mentioned underpressure distillation is to reclaim dimethyl carbonate under nitrogen, carbon dioxide and argon protection.

Main advantages and positive effects of the present invention:

(1) The solvent dimethyl carbonate used in the present invention overcomes the unavoidable residual problem of organic solvents in the existing solvents for extracting total flavonoids of jasmine, so dimethyl carbonate is used as a solvent to produce total flavonoids of jasmine without polluting the product. It does not pollute the environment and is more in line with the safety requirements of medicines. The explosion limit of dimethyl carbonate is 3.8-21.3%. Using it as a leaching solvent greatly reduces the danger in production and realizes production safety. At the same time, dimethyl carbonate has no health problems for operators. It is a kind of Inexpensive green solvent that combines cleanliness and safety.

(2) The extruder, crusher or roller machine used in the present invention crushes jasmine flowers, stems or leaves, so that the active ingredients of jasmine can be extracted quickly, energy consumption is reduced, and the product yield is higher.

(3) The ultrasonic technology that the present invention adopts extracts, has utilized the cavitation effect of ultrasonic wave to accelerate the stripping of active ingredient of plant, utilizes the secondary effect of ultrasonic wave in addition, as mechanical vibration, diffusion, crushing, chemical effect etc., can also accelerate jasmine The active ingredient is diffused and released and fully mixed with the solvent, which is conducive to complete extraction, and the product yield reaches 98.6%.

(4) The present invention impregnates the raw materials, and the raw materials are first wetted and then extracted, which solves the technical problems that the solvent is difficult to penetrate and the active ingredients are difficult to export.

(5) The present invention uses response surface analysis (RSM) based on the regression relationship between several variables and one or more dependent variables, and obtains the regression relationship optimization of extraction conditions and extraction results through regression analysis, thereby determining the best extraction The process is as follows: solvent pH value 5.5-6, liquid-solid ratio 15-20:1, raw material immersion for 10-20 minutes, extraction temperature 85-92°C, ultrasonic extraction time 20-30 minutes, natural chromatography 0.5-1 hour.

(6) The method of the present invention has short technological process, easy operation, short extraction time, less solvent loss, energy saving and environmental protection, high product yield, low product cost, greatly reduces the risk in production, and has good economic benefits and social benefits. benefits and ecological benefits.

detailed description

Below in conjunction with specific embodiment, the present invention will be further described, and the present invention is not limited to following embodiment, and the embodiment enumerated is only the specific method of the present invention, and those of ordinary skill in the art can directly derive or associate from the disclosed content of the present invention All the deformations obtained should be considered as the protection scope of the present invention.

Example 1

A method for optimizing the extraction of total flavonoids from jasmine by response surface methodology, the process steps are:

(1) Raw material crushing: crush the jasmine flower crusher;

(2) Impregnation: Put 50 kg of crushed jasmine into the extraction tank, then add 1000 kg of dimethyl carbonate solvent with a pH value of 6, and impregnate for 10 minutes;

(3) Extraction: after immersion, heat up to 85°C, start ultrasonic, control the frequency to 40 kHz, and control the time for 30 minutes, filter, re-extract the filter residue once, and combine the filtrate;

(4) Separation: put the combined filtrate of step (3) in a chromatographic tank for natural chromatography for 1 hour, then discharge the solvent and continue to use in the next batch of production;

(5) Purification: Add the extract of total flavonoids of jasmine separated in step (4) into a purification tank, continue natural chromatography, and filter to obtain the total flavonoids of jasmine. The product extraction rate is 99.1%.

Example 2

A method for optimizing the extraction of total flavonoids from jasmine by response surface methodology, the process steps are:

(1) Crushing of raw materials: crushing jasmine stems with a roller press;

(2) Impregnation: Put 50 kg of broken stems into the extraction tank, then add 750 kg of dimethyl carbonate solvent with a pH value of 5.5, and impregnate for 20 minutes;

(3) Extraction: After immersion, heat up to 92°C, start ultrasonic wave, control the frequency to 40 kHz, and control the time for 25 minutes, filter, re-extract the filter residue twice, and combine the filtrate;

(4) Separation: put the combined filtrate of step (3) into a chromatographic tank for natural chromatography for 0.8 hours, then discharge the solvent and continue to use it for the next batch of production;

(5) Purification: Add the extract of total flavonoids of jasmine separated in step (4) into a purification tank, continue natural chromatography, and filter to obtain the total flavonoids of jasmine. The product extraction rate is 98.6%.

Example 3

A method for optimizing the extraction of total flavonoids from jasmine by response surface methodology, the process steps are:

(1) Crushing of raw materials: crushing jasmine leaves with an extruder;

(2) Impregnation: Put 50 kg of broken jasmine leaves into the extraction tank, then add 900 kg of dimethyl carbonate solvent with a pH value of 5.8, and impregnate for 15 minutes;

(3) Extraction: After immersion, under the condition of raising the temperature to 90°C, start the ultrasonic wave, control the frequency to 48 kHz, and control the time for 20 minutes, filter, re-extract the filter residue once, and combine the filtrate;

(4) Separation: put the combined filtrate of step (3) in a chromatography tank for natural chromatography for 0.5 hours, and discharge the solvent to continue to be used in the next batch of production;

(5) Purification: Add the extract of total flavonoids of jasmine separated in step (4) into a purification tank, continue natural chromatography, filter out and then use conventional vacuum distillation to obtain total flavonoids of jasmine. The product extraction rate is 98.8%.

Claims (4)

1. a kind of method that jasmine general flavone is extracted in response phase method optimization, it is characterised in that：Using design expert softwares, The liquid that the solution pH, temperature, time and the solvent that extract jasmine general flavone and raw material jasmine are designed according to Box-Behnken is solid Than process conditions, jasmine general flavone, including following technological operation step are extracted with ultrasonic assistant：

(1) raw material is crushed：Jasmine, stem and leaf are crushed respectively, it is standby；

(2) impregnate：Broken Jasmine, stem or leaf are put into extractor, and solvent, leaching are added with liquid-solid ratio 15~20: 1 Stain 10~20 minutes；

(3) extract：It is warming up to after dipping under conditions of 85~92 DEG C, starts ultrasonic wave, control time 20~30 minutes is filtered, Extraction time is 2~3 times, merging filtrate；

(4) separate：Will step (3) merging filtrate place nature chromatography tank in chromatograph naturally 0.5~1 hour, discharge solvent after Continue for next group production solvent；

(5) purify：The jasmine general flavone extract solution that step (4) is separated is added in purifying tank, is continued nature and is chromatographed, filtering, or Person uses vacuum distillation, obtains jasmine general flavone product；

Described solvent is dimethyl carbonate, and solution pH 5.5~6 is adjusted with hydrochloric acid, acetic acid or sodium hydroxide；

Described ultrasonic wave controls frequency to be 40~50kHz.

2. the method that jasmine general flavone is extracted in a kind of response phase method optimization according to claim 1, it is characterised in that：It is described Broken selection extruder, disintegrating machine or roller machine.

3. the method that jasmine general flavone is extracted in a kind of response phase method optimization according to claim 1, it is characterised in that：It is described Vacuum distillation be nitrogen, carbon dioxide and argon gas protection under carry out recovery dimethyl carbonate.

4. the method that jasmine general flavone is extracted in a kind of response phase method optimization according to claim 1, it is characterised in that：Including Following technological operation step：

(1) raw material is crushed：Jasmine disintegrating machine is crushed；

(2) impregnate：By in broken 50 kilograms of input extractors of Jasmine, the dimethyl carbonate solvent of pH value 6 is added 1000 kilograms, impregnate 10 minutes；

(3) extract：85 DEG C are warming up to after dipping, starts ultrasonic wave, it is 40kHz to control frequency, control time 30 minutes is filtered, Cross filter residue and bring up again and take 1 time, merging filtrate；

(4) separate：The merging filtrate of step (3) is placed into chromatography tank to chromatograph naturally 1 hour, is then discharged out under solvent continues on for A collection of production；

(5) purify：The jasmine general flavone extract solution that step (4) is separated is added in purifying tank, continues nature chromatography, and filtering is obtained To jasmine general flavone product.