CN1757642A - Method for preparing soyabean dregs isoflavone - Google Patents

Abstract

This invention relates to a preparation method for a kind of soy isoflavone, particularly an extraction process for soy isoflavone product with de-fat soy home produced non-transgenic soybean as raw material, with physical and chemical measure including extraction, concentration, hydrolysis, separation. purification, spray drying etc. process, first continuously reflex extracting soy with ethanol aqueous solution to obtain active substance extraction solution, vaporizing under vacuum to obtain concentrated solution, mixing the concentrated solution and alkaline liquid in a reactor, stirring continuously under controlled temperature to go through hydrolysis reaction; after regulating pH number reaction of the solution with aqueous hydrogen chloride, through centrifugal separation initial extraction of isoflavone is produced, after washing the initial extraction substance with water, then recrystallized in aqueous ethanol and spray dried the product isoflavone is formed. The technical route of the process of this invent is simple and easy, the equipment is available, it has easy controlled condition, low energy consumption, high extraction yield, good quality, it may effectively extract content of isoflavone in soybean.

Description

The preparation method of bean mill cake isoflavone

Technical field:

The present invention relates to a kind of preparation method of bean mill cake isoflavone, defatted soybean meal with homemade non-transgenic soybean is that raw material adopts physics and chemical means, through technological processs such as extraction, hydrolysis reaction, separation, refining, spraying dryings, realize the production of soybean isoflavones, particularly a kind of processing method of ethanol water duo-sol extraction bean mill cake isoflavone.

Technical background:

Soybean is one of agricultural planting oil crops of the maximum of production and consumption amount in the world, plants with a long history.Because of its high protein, low-cholesterol is rich in biologically active substances such as female hormone, has remarkable nutritive value, is subjected to liking of the people of the world.Report explanation is arranged, Asia climacteric syndrome degree is low be because of human consumption soybean and goods thereof more than other countries.2,500 ten thousand tons of China annual consumption soybean.Dregs of beans after the oil expression all uses as feed and fertilizer.The albumen that contains in the dregs of beans after the oil expression, isoflavones, oligose, the contour using value of saponin and economic worth have caused entrepreneur and scientist's extensive concern.China begins plantation at first, and finds its nutritive value and as the nationality of protein source.Moreover, according to historical records, legendary god of farming emperor classified soybean one of as five cereals at that time; The medicinal herbs scholar in ancient times mentions its curative effect widely, comprises that at diseases such as kidney disease, tetter, vitamin B1 deficiency, diarrhoea, blood viral disease, constipation, anemias good curative effect is all arranged.

Soybean isoflavones is one of the most compelling functional active components in the soybean.Soybean isoflavones is a class secondary metabolite that forms in the soybeans they grow, is a kind of in the biological flavone, also is a kind of phytoestrogen.The content of soybean isoflavones is 0.4%-0.6% in the soybean.Do not contain soybean isoflavones in the soybean oil, so defatted soybean meal is the important source of soybean isoflavones.As far back as in January, 1999, the american cancer research centre, the natural active matter of inviting many famous experts to study in the soybean has in the anticancer effect meeting, oestrogenic hormon in the brainstrust abundant affirmation soybean isoflavones is anti-cancer, anticancer effective active substance, and definite soybean isoflavones has stronger physiological property, is healthcare products and the valuable added ingredientss of medicine.Therefore, be widely used in protective foods and medicine and other fields.Whole world soybean consumption is big, but utilization ratio is low.In recent years, the functional activity composition that is rich in the soybean and its effect, excited scientist and entrepreneur, the wide market outlook that also indicating the natural function product of soybean isoflavones isoreactivity composition.The soybean consumption that China is annual 2500 ten thousand tons, its effect only is edible oil, feed and fertilizer.It has been found that the bioactive ingredients of soybean, its extracting method of exploitation that also begins one's study, but safety, efficient, low consumption, industrialization, commercial Appropriate technology form as yet.

Because the physiological function of the functional activity composition that is rich in the soybean meal receives global concern, the healthcare products in the whole world and the demand of pharmaceuticals will grow with each passing day, so develop industrialized manufacturing technique and device, have important society and economic worth from soybean dregs of beans extraction functionality activeconstituents soybean isoflavones.Adopting the extraction process technology of safety non-toxic, produce the high inexpensive biologically active native functional product of matter, will be the requirement of soybean deep processing industry development.

Commercial processes route from soybean dregs of beans extraction functionality activeconstituents soybean isoflavones mainly contains methanol solvate extraction method, ethyl acetate solvent extraction method, alkali liquor extraction method, macroreticular resin absorbing method etc.In the early stage production at home and abroad, mainly adopt the extracting method of first three kind.Because have dissolvent residual, poor stability, problems such as yield is low, energy consumption is big, molten consumption height, heavy metal excess, people focus on sight on the macroreticular resin absorbing method of excellent property again.Consider that the security of the biological activity goods that macroporous adsorbent resin extracts does not obtain the confirmation of scientific circles as yet, Ministry of Health of the People's Republic of China issues an order: the functional activity composition of forbidding extracting with macroporous resin adsorption is as healthcare products and medical raw material.At present, the new production technique of domestic positive active development is extracted the functional activity composition soybean isoflavones in the soybean meal.The patent that obtains about the production technique from soybean dregs of beans extraction functionality activeconstituents soybean isoflavones mainly concentrates on the alkali liquor extraction method in the world.

End is got up, and extracts at present in the processing method of bean mill cake isoflavone ubiquity and complex technical process from soybean, and technological principle is outmoded, and use equipment and technology condition are loaded down with trivial details, big energy-consuming, and product goes out shortcomings such as rate is low.

Summary of the invention:

The objective of the invention is to overcome the shortcoming that exists in the prior art, seek to design a kind of processing method of utilizing the dual solvent of second alcohol and water from not genetically modified skimmed soy beans dregs of beans, to extract isoflavones components.

In order to realize the foregoing invention purpose, technological processs such as Technology of the present invention comprises extraction, concentrates, hydrolysis reaction, separate and subside, refining, spraying drying.At first adopt 60～80% aqueous ethanolic solution that homemade non-transgenic skimmed soy beans dregs of beans is carried out counter current continuous extraction, extract active substance mixed solution wherein, as materials such as soybean isoflavones, soybean oligosaccharide and saponins; The negative pressure evaporation concentrated extracting solution obtains concentrated solution.Concentrated solution and certain density alkali lye are mixed in the reactor, temperature control between 50～90 ℃, continuously stirring, hydrolysis reaction carries out certain hour, concentration of lye wherein is 1mol/L to 10mol/L; Temperature control adopts certain density hydrochloric acid soln to transfer the potential of hydrogen of reaction solution to certain value again, and its pH value scope is reacted between 8 to 4; Centrifugation is separated out the primary extract of soybean isoflavones, and again after water washing, recrystallization and carry out spraying drying in conventional equipment in ethanol water solvent obtains the soybean isoflavones product.Detect through high pressure liquid chromatography (HPLC), determine its isoflavone content.

Adopt this processing method to produce the soybean meal isoflavones, it has, and operational path is simple, and equipment is easy to get, and control condition is convenient, and energy consumption is low, and product goes out the rate height, outstanding advantage such as quality better.

Specific embodiments:

The present invention can be specifically described its preparation process and effect by following embodiment.

Embodiment 1:

One, homemade not genetically modified skimmed soy beans dregs of beans during the selected raw material of technological experiment adopts.

Two, ethanolic soln counter current continuous extraction under 45-50 ℃ of service temperature of 75% is adopted in extraction in conventional equipment, negative pressure evaporation, and obtaining concentrated solution is 20% of total charging capacity.Detect through high pressure liquid chromatography (HPLC), the content of soybean isoflavones is 0.8% in this concentrated solution.

Three, in proportion (concentrated solution: water=1: 3) be mixed with solution, 75 ℃ of stirrings of temperature control in reactor are 12 with 2mol/L sodium hydroxide (NaOH) solution adjust pH, decomposition reaction 90 minutes.

Four, temperature control is 50 ℃, with concentration be hydrochloric acid (HCl) solution of 2mol/L to transfer pH be 5, reacted 60 minutes, centrifugation soybean crude extract 1 wherein contains soybean isoflavones 4-6%, yield 40-50%.Liquid phase continues to stir 50 ℃ of temperature controls, and 60 minutes, centrifugation soybean crude extract 2 wherein contained soybean isoflavones 1.5-2.5%, and yield is 40-50%.Merge two step total yields and reach 80-90%.

Five, to crude extract 1 and crude extract 2 merge adopt washing after, refining with a spot of anhydrous alcohol solution, filter particulate crystal isoflavones, through conventional equipment and condition spray drying treatment, get content greater than 40% isoflavones product.The experiment product is analyzed through high pressure liquid chromatography (HPLC), and isoflavones purity reaches 70%.

Repeatedly test by above-mentioned steps, its result is identical, illustrates that its operational path and conditionally complete are suitable for producing in batches.

Claims (3)

1, a kind of preparation method of bean mill cake isoflavone, comprise extraction, concentrate, hydrolysis reaction, separate and subside, refining, drying process with atomizing process, it is characterized in that adopting aqueous ethanolic solution that dregs of beans is carried out counter current continuous extraction earlier gets the active substance extracting solution, gets concentrated solution to the extracting solution negative pressure evaporation; Concentrated solution and alkali lye are mixed in the reactor reaction that is hydrolyzed of temperature control continuously stirring; Temperature control and to transfer the pH value of the potential of hydrogen of reaction solution with hydrochloric acid soln be to react between 8 to 4 again; Centrifugation analyse isoflavone primary extract; To primary extract after washing in ethanol water solvent recrystallization and spraying drying get the isoflavones product;

2, the preparation method of bean mill cake isoflavone according to claim 1, the aqueous ethanolic solution concentration that it is characterized in that extracting usefulness is 60～80%; The mixed alkali liquor concentration that adds in the reactor be 1mol/L to 10mol/L, its temperature control scope is between 50～90 ℃;

3, the preparation method of bean mill cake isoflavone according to claim 1 is characterized in that again control temperature is 50 ℃, and the concentration of hydrochloric acid soln is the potential of hydrogen that the condition of 2mol/L is transferred reaction solution.