CN105524035A - Manufacturing method of mulberry anthocyanidin - Google Patents

Abstract

The invention belongs to the field of natural organic chemistry and relates to extraction and separation method of anthocyanidin from mulberry. According to the method, tea polyphenol which is used as an antioxidant is extracted under the alkaline condition; impurities are removed by the use of a flocculant under the acidic condition; and an extracting solution is purified by the use of cation exchange resin so as to obtain a high-purity anthocyanidin product. The invention has advantages as follows: 1, as water is used as an extraction solvent under the alkaline condition, production cost is greatly reduced by the method in comparison with a traditional extraction method by the use of ethanol; 2, by adding a natural antioxidant in the extraction process, loss of anthocyanidin can be effectively reduced; 3, impurities in the extracting solution are deposited by the use of a flocculant; and 4, the extracting solution is purified by the use of cation exchange resin so as to remarkably raise purity of the anthocyanidin product. The prepared anthocyanidin can be widely applied in fields of health food and cosmetic, etc.

Description

A kind of manufacture method of mulberries anthocyanidin

Technical field

The invention belongs to field of natural organic chemistry, relating to a kind of take mulberries as the industrial method that anthocyanidin prepared by raw material.

Background technology

Anthocyanidin is a kind of water colo(u)r, can change color along with the soda acid of enchylema.Enchylema is that acidity is then partially red, and enchylema is that alkalescence is then partially blue, and anthocyanidin is one of primary pigments forming petal and fruit color.Anthocyanidin is plant secondary metabolism product, physiology is played the part of important role, anthocyanidin is the antidotal nutritious supplementary of pure natural, research proves mankind nowadays and finds the most effective anioxidant phytochemicals, its antioxidant property exceeds 50 times than vitamin-E, exceeds 20 times than vitamins C.It is 100% to the biological effectiveness of human body, within 20 minutes, just can detect in blood after taking, to vision enhancing, anti-eye strain, delay cranial nerve aging and have significant effect, also there is better therapeutic action to the microangiopathy caused by diabetes simultaneously, the various diseases such as cardio-pulmonary function, prevention senile dementia can also be strengthened.

(s ā ngshen reads again s ā ngren to mulberries ^[1]), the mature fruit of mulberry tree, mulberries are again sorosis, mulberry bubble youngster, and peasant likes the fresh fruit of its maturation to eat, and taste sweet juice is many, is one of fruit of often eating of people, wherein containing a large amount of anthocyanidin.

Extracting method conventional at present has: organic solvent extraction, supercritical extraction, microwave method and ultrasonic extraction.Organic solvent extraction is common extraction anthocyanidin method, after complete with solvent extraction, needs with extractions such as some organic solvents such as sherwood oil, just own institute, ether to remove the lipid-soluble substance in crude extract.The advantage of organic solvent extraction is easy and simple to handle, does not need complicated plant and instrument; Shortcoming is that organic solvent consumption is high, time-consuming, and will heat the oxidative degradation that can cause anthocyanidin when extracting.Microwave method and supersonic method, due to the limit value of equipment, also cannot carry out large-scale industrial production.Supercritical extraction can realize industrialization at present, but due to the singularity of this technology, the anthocyanidin causing utilizing this technology to produce is with high costs, cannot by this product promotion in ordinary consumer.

Purification process comparatively conventional at present mainly adopts macroporous adsorbent resin to carry out, and the advantage of macroporous adsorbent resin is that adsorptive capacity is large, can recycle, can be cost-saving on certain cost; Shortcoming is that the impurity of absorption is also many, and it is not very remarkable that the product purity after purifying promotes.

Summary of the invention

The object of the present invention is to provide a kind of industrial method preparing mulberries anthocyanidin from mulberries.The present invention first adopts alkaline aqueous solution to extract under the existence of natural antioxidants, and recycling flocculation agent carries out removal of impurities under weakly acidic condition, then utilizes Zeo-karb to carry out separation and purification, obtains highly purified anthocyanidin product.

Technical scheme of the present invention is achieved in that it comprises the following steps:

(1) extract: the alkaline aqueous solution being 10 ~ 12 by practical for mulberries pH value extracts under natural antioxidants existent condition, obtains the extracting solution containing anthocyanidin;

(2) acidifying: add acidic aqueous solution in extracting solution, makes the pH value of extracting solution maintain between 6 ~ 7;

(3) removal of impurities: add a certain amount of flocculation agent in extracting solution, leaves standstill after stirring under certain condition, then by centrifugal segregation solid substance impurity wherein, obtains solution;

(4) purifying: first adsorbed with Zeo-karb by solution, then carries out wash-out with acidic solution to Zeo-karb, obtains the solution containing anthocyanidin;

(5) concentrated; Solution basic solution being adjusted to pH value is 4 ~ 6, then carries out concentrating under reduced pressure, obtains concentrated solution;

(6) dry: concentrated solution adopts spraying dry, obtains mulberries anthocyanidin product;

In described step (1), natural antioxidants comprises one or more in vitamin A, C, E, P, polyphenol, vegetable active selenium, usage quantity is 0.1 ~ 1% of mulberries raw materials quality, Extracting temperature is 70 ~ 80 DEG C, raw material: extracting solution=1: 5 ~ 10 (m/v), extraction time is 60 ~ 120min;

In described step (3), described flocculation agent is ZTC1+1 type, addition 2%, temperature 40 DEG C, stirs 5min, then leaves standstill 120min, centrifuge;

In described step (4), the centrifugate Zeo-karb of step (3) gained is carried out purifying, the upper column flow rate of centrifugate is 1BV/h, then uses deionized water rinsing, and flow velocity is 1.5BV/h, and the consumption of deionized water is 2BV; Then carry out wash-out with the aqueous hydrochloric acid of 2 ~ 5%, the flow velocity of elutriant is 1.5BV/h, and the consumption of elutriant is 3 ~ 5BV.

Embodiment

Embodiment 1

Dropped in extractor by the Extraction solvent buck (pH=12) of the mulberries of 1000kg and 5000kg, and in extractor, drop into the vitamins C that 5kg purity is 95%, Extracting temperature is 70 DEG C, and extraction time is 90min, extracts 2 times, collects extracting solution; Adopt acidic aqueous solution (pH=1) to regulate the extracting solution collected, making it pH value is 6.4, then adds ZTC1+1 type flocculation agent wherein, addition 2%, stirs 5min under the condition of temperature 40 DEG C, then leaves standstill 120min, centrifuge, collects centrifugate; Centrifugate 001 type Zeo-karb is carried out purifying, the upper column flow rate of centrifugate is 1BV/h, use deionized water rinsing again, flow velocity is 1.5BV/h, the consumption of deionized water is 2BV, then carries out wash-out with the aqueous hydrochloric acid of 4.5%, and the flow velocity of elutriant is 1.5BV/h, the consumption of elutriant is 5BV, obtains the elutriant containing anthocyanidin.Elutriant alkaline aqueous solution is readjusted prices pH value between 4 ~ 6, then vacuum-concentrcted, vacuum tightness is-0.08 ~ ~ 0.07Mpa, and thickening temperature is at 50 ± 2 DEG C, and recycling design, obtains enriched material; Utilized by enriched material spray-dryer to carry out drying again, inlet temperature is 200 ~ 210 DEG C, and temperature out is 80 ~ 90 DEG C, obtains the mulberries anthocyanidin product 5.21kg that anthocyanidin content is 27.3%.

Embodiment 2

Dropped in extractor by the Extraction solvent buck (pH=11) of the mulberries of 1000kg and 5000kg, and in extractor, drop into the vitamin-E that 10kg purity is 50%, Extracting temperature is 75 DEG C, and extraction time is 120min, extracts 2 times, collects extracting solution; Adopt acidic aqueous solution (pH=1) to regulate the extracting solution collected, making it pH value is 6.7, then adds ZTC1+1 type flocculation agent wherein, addition 2%, stirs 5min under the condition of temperature 40 DEG C, then leaves standstill 120min, centrifuge, collects centrifugate; Centrifugate D-85 macropore propionic acid alkene system weakly acidic cation-exchange resin is carried out purifying, the upper column flow rate of centrifugate is 1BV/h, use deionized water rinsing again, flow velocity is 1.5BV/h, the consumption of deionized water is 2BV, then carries out wash-out with the aqueous hydrochloric acid of 3.0%, and the flow velocity of elutriant is 1.5BV/h, the consumption of elutriant is 4.5BV, obtains the elutriant containing anthocyanidin.Elutriant alkaline aqueous solution is readjusted prices pH value between 4 ~ 6, then vacuum-concentrcted, vacuum tightness is-0.08 ~-0.07Mpa, and thickening temperature is at 50 ± 2 DEG C, and recycling design, obtains enriched material; Utilized by enriched material spray-dryer to carry out drying again, inlet temperature is 200 ~ 210 DEG C, and temperature out is 80 ~ 90 DEG C, obtains the mulberries anthocyanidin product 5.34kg that anthocyanidin content is 25.3%.

Claims (1)

1. a manufacture method for mulberries anthocyanidin, it comprises the following steps:

(1) extract: the alkaline aqueous solution being 10 ~ 12 by practical for mulberries pH value extracts under natural antioxidants existent condition, obtains the extracting solution containing anthocyanidin;

(2) acidifying: add acidic aqueous solution in extracting solution, makes the pH value of extracting solution maintain between 6 ~ 7;

(3) removal of impurities: add a certain amount of flocculation agent in extracting solution, leaves standstill after stirring under certain condition, then by centrifugal segregation solid substance impurity wherein, obtains solution;

(4) purifying: first adsorbed with Zeo-karb by solution, then carries out wash-out with acidic solution to Zeo-karb, obtains the solution containing anthocyanidin;

(5) concentrated: solution basic solution being adjusted to pH value is 4 ~ 6, then carries out concentrating under reduced pressure, obtains concentrated solution;

(6) dry: concentrated solution adopts spraying dry, obtains mulberries anthocyanidin product;

In described step (1), natural antioxidants comprises one or more in vitamin A, C, E, P, polyphenol, vegetable active selenium, usage quantity is 0.1 ~ 1% of mulberries raw materials quality, Extracting temperature is 70 ~ 80 DEG C, raw material: extracting solution=1: 5 ~ 10 (m/v), extraction time is 60 ~ 120min;

In described step (3), described flocculation agent is ZTC1+1 type, addition 2%, temperature 40 DEG C, stirs 5min, then leaves standstill 120min, centrifuge;

In described step (4), the centrifugate Zeo-karb of step (3) gained is carried out purifying, the upper column flow rate of centrifugate is 1BV/h, then uses deionized water rinsing, and flow velocity is 1.5BV/h, and the consumption of deionized water is 2BV; Then carry out wash-out with the aqueous hydrochloric acid of 2 ~ 5%, the flow velocity of elutriant is 1.5BV/h, and the consumption of elutriant is 3 ~ 5BV.