CN103694294A - Method for extracting baicalin by use of flash extraction technology - Google Patents

Abstract

The invention discloses a method for extracting baicalin by use of a flash extraction technology, which comprises the steps of firstly putting radix scutellariae pieces into an extraction pot, and adding ethanol 10 times the radix scutellariae pieces in quantity; starting a flash extractor for extraction, and filtering; concentrating the filtrate and recycling the ethanol to obtain a crude extract of baicalin; adding purified water 15 times the crude extract in quantity, heating to 80 DEG C and stirring into a suspension; adjusting the pH value with hydrochloric acid to 1-2; preserving heat and standing and discarding the supernate; adjusting the pH value with a sodium hydroxide solution to 7.0; adding ethanol of equal quantity, stirring for dissolution and filtering; adjusting the pH value of the filtrate with hydrochloric acid to 1.0-2.0; preserving heat and standing for one hour at 60-85 DEG C so that the baicalin is separated by crystallization; filtering with filter paper; washing with ethanol until the pH value is 5.0-7.0; washing with purified water and drying to obtain a finished product of baicalin with purity of 87-89.5%. As the flash extraction technology is applied to the baicalin extraction method, compared with the traditional method, the method disclosed by the invention has the advantages that the purity of the extracted baicalin is high, the yield is high, the extraction time is short, and the process is simple and easy to operate.

Description

Utilize and dodge the method that the technology of putting forward is extracted baicalin

Technical field

The present invention relates to the extracting method of baikal skullcap root, especially relate to a kind of utilization and dodge the method that the technology of putting forward is extracted baicalin.

Background technology

The root of large-flowered skullcap is a kind of conventional Chinese medicine, and baicalin Baicalin is present in the root of dicotyledons Labiatae Labiatae root of large-flowered skullcap Scutellaria baicalensis Georgi in a large number.Baicalin is the crystalline powder of faint yellow fine needle, belongs to flavonoid; Fusing point 223-225 ℃, [α] 18D+123 ℃ (c=0.2, pyridine-water); Be soluble in DMF, in pyridine, dissolve in the basic solutions such as sodium bicarbonate, sodium carbonate, sodium hydroxide, but unstable in alkali lye, crossfade into burgundy, be slightly soluble in hot Glacial acetic acid, be insoluble in formic acid, acetic acid, acetone, hardly water-soluble, ether, benzene, chloroform etc.Baicalin has significant biological activity, has antibacterial, diuresis, anti-inflammatory, resistance state and spasmolysis, and has the stronger physiological potencies such as antitumor response, has occupied critical role on clinical medicine.Baicalin can also absorb ultraviolet ray, removes oxyradical, and generation that again can check melanin, therefore both can be used for medicine, also can be used for makeup, was a kind of good functional cosmetics raw material.

At present from the root of large-flowered skullcap, extract the method that baicalin is conventional and mainly contain solvent-extraction process, ultrasonic extraction, ultrafiltration extraction method, microwave extraction method and supercritical extraction method etc.Conventional extraction process is that water extraction, acid are heavy, filtration, alkali are molten, carry out acid again sinks, and decocting boils root of large-flowered skullcap meal twice, and acid adding is adjusted to pH 1～2,70～80 ℃ of insulations, standing 12～24h, filters, and throw out adds water and stirs into suspension, with adjusting PH with base 7～7.5 to after dissolving, add ethanol and stir, filter, then acid adding is adjusted pH 1～2,80 ℃ of insulations, obtain baicalin crystallization.The whole leaching process cycle is longer, has both consumed the energy, and the three wastes of generation are also a lot.Simultaneously because baicalin is water-soluble hardly, even heated and boiled, the solubleness of baicalin is still very low, so it is very low to extract in this way baicalin yield, only can reach 10% left and right, heating not only causes the waste of mass energy, hot water extraction also can increase the stripping of other impurity simultaneously, post-processed is more difficult, causes baicalin purity lower, is only below 85%.

It is a kind of novel extractive technique that technology is put forward in sudden strain of a muscle, has extract at room temperature, rapidly and efficiently, does not destroy effective constituent, the advantage such as energy-saving and cost-reducing, easy and simple to handle, and 200Duo Jia plant research mechanism and scientific research institutions are widely used at home at present; The flash extracter of proposing technological invention according to sudden strain of a muscle has been awarded utility model patent (patent No. is: ZL2005 2 0031604.9) in 2006.But adopt to dodge the technology of putting forward and extract the method for baicalin so far there are no report.

Summary of the invention

The object of the present invention is to provide a kind of utilization to dodge the method that the technology of putting forward is extracted baicalin, the method can make the total recovery of baicalin reach 17.1%.

For achieving the above object, the present invention can take following technical proposals:

The method that the technology of putting forward is extracted baicalin is dodged in utilization of the present invention, comprises the steps:

The first step, puts into extractor by baikal skullcap root decoction pieces, adds the ethanol of 10 times of amounts of baikal skullcap root decoction pieces, starts flash extracter and extracts 5 minutes, filters and obtains filtrate;

Second step, after using conventional thickening equipment to concentrate filtrate, reclaims ethanol, obtains baicalin crude extract medicinal extract;

The 3rd step, adds the pure water of 15 times of amounts of crude extract medicinal extract, is heated to 80 ℃ and stir and make it to become suspension, with concentrated hydrochloric acid, regulates pH value to 1.0 ~ 2.0, is incubated standing 1 h, abandoning supernatant; 40% sodium hydroxide solution for suspension is adjusted to pH to 7.0, then add the ethanol with content equivalent, stir and make it to dissolve, filter; Filtrate is used hydrochloric acid adjust pH to 1.0 ~ 2.0,60 ~ 85 ℃ of standing 1h of insulation, baicalin crystallization;

The 4th step, filter paper filtering is first used in the baicalin crystallization that the 3rd step is obtained, and with ethanol, is washed till pH 5.0 ~ 7.0, and then with pure water washing 3 ~ 4 times, proceeds to 120 ~ 150 ℃ of oven dry of baking oven, can obtain purity and reach 89.5 ~ 91.0% baicalin finished product.

For reaching better extraction effect, the concentration of ethanol used is 65%(volume ratio).

The invention has the advantages that sudden strain of a muscle is put forward to technology to be applied in the method for extracting baicalin, compares the baicalin purity high (reaching 89.5 ~ 91.0%) of extraction, yield high (reaching 17.1%) with traditional method; Extraction time is reduced to about 3 hours from being greater than 24 hours, greatly shortened extraction time, and all processes is simple to operation, during extraction, do not make water make solvent, do not heat, only use ethanol as extracting solvent, easily reclaim and can reuse, extraction cost is lower, is more conducive to environmental protection, more energy-saving and cost-reducing.

Embodiment

The method that the technology of putting forward is extracted baicalin is dodged in utilization of the present invention, comprises the steps:

The first step, puts into extractor by baikal skullcap root decoction pieces, adds the ethanol (best results while experiment showed, the extraction using alcohol of concentration 65%) of 10 times of amounts of baikal skullcap root decoction pieces, starts flash extracter and extracts 5 minutes, filters and obtains filtrate;

Second step, after using conventional thickening equipment to concentrate filtrate, reclaims ethanol, obtains baicalin crude extract medicinal extract;

The 3rd step, adds the pure water of 15 times of amounts of crude extract medicinal extract, is heated to 80 ℃ and stir and make it to become suspension, and salt acid for adjusting pH value to 1.0 ~ 2.0 with 2mol/L, are incubated standing 1 h, abandoning supernatant; 40% sodium hydroxide solution for suspension is adjusted to pH to 7.0, then add the ethanol with content equivalent, stir and make it to dissolve, filter; Filtrate is used hydrochloric acid adjust pH to 1.0 ~ 2.0 of 2mol/L, 60 ~ 85 ℃ of standing 1h of insulation, baicalin crystallization;

The 4th step, filter paper filtering is first used in the baicalin crystallization that the 3rd step is obtained, and the ethanol with 65% is washed till pH 5.0 ~ 7.0, and then with pure water washing 3 ~ 4 times, proceed to 120 ~ 150 ℃ of oven dry of baking oven and (experiment showed, when bake out temperature is too low, drying time is longer, waste electric energy; Bake out temperature is too high, can cause baicalin variable color sex change etc.), can obtain purity and reach 89.5 ~ 91.0% the crystalline baicalin finished product of faint yellow fine needle powder, baicalin total recovery can reach 17.1%.

Claims (2)

1. utilize and dodge the method that the technology of putting forward is extracted baicalin, it is characterized in that: comprise the steps:

The first step, puts into extractor by baikal skullcap root decoction pieces, adds the ethanol of 10 times of amounts of baikal skullcap root decoction pieces, starts flash extracter and extracts 5 minutes, filters and obtains filtrate;

Second step, after using conventional thickening equipment to concentrate filtrate, reclaims ethanol, obtains baicalin crude extract medicinal extract;

The 3rd step, adds the pure water of 15 times of amounts of crude extract medicinal extract, is heated to 80 ℃ and stir and make it to become suspension, with concentrated hydrochloric acid, regulates pH value to 1.0 ~ 2.0, is incubated standing 1 h, abandoning supernatant; 40% sodium hydroxide solution for suspension is adjusted to pH to 7.0, then add the ethanol with content equivalent, stir and make it to dissolve, filter; Filtrate is used hydrochloric acid adjust pH to 1.0 ~ 2.0,60 ~ 85 ℃ of standing 1h of insulation, baicalin crystallization;

The 4th step, filter paper filtering is first used in the baicalin crystallization that the 3rd step is obtained, and with ethanol, is washed till pH 5.0 ~ 7.0, and then with pure water washing 3 ~ 4 times, proceeds to 120 ~ 150 ℃ of oven dry of baking oven, can obtain purity and reach 89.5 ~ 91.0% baicalin finished product.

2. the method that the technology of putting forward is extracted baicalin is dodged in utilization according to claim 1, it is characterized in that: in the first step, the concentration of ethanol used is 65%.