阅读说明：本技术 一种红树莓花青素的提取方法 (Extraction method of red raspberry anthocyanin ) 是由 叶红玲 刘冬 姚军 吕新霞 哈满林 于 2021-07-07 设计创作，主要内容包括：本发明公开了一种红树莓花青素的提取方法,涉及花青素提取领域,以清理去杂后的红树莓为原料,经打浆、超声提取、离心、浓缩、吸附、洗脱、浓缩、干燥提取花青素,打浆机与超声波提取器使红树莓细胞壁破碎,其中的花青素暴露于有机溶剂中,离心将细胞中的其余物质与溶有花青素的溶液分离,减压浓缩后得到粗提液,再将粗提液过滤吸附后洗脱收集,浓缩干燥后得到花青素,采用一体式红树莓花青素提取设备,提高提取率,降低人工成本。(The invention discloses a method for extracting anthocyanin from red raspberries, which relates to the field of anthocyanin extraction, wherein the red raspberries after being cleaned and decontaminated are taken as raw materials, the anthocyanin is extracted by beating, ultrasonic extraction, centrifugation, concentration, adsorption, elution, concentration and drying, the cell walls of the red raspberries are crushed by a beating machine and an ultrasonic extractor, the anthocyanin is exposed in an organic solvent, the rest substances in cells are separated from a solution dissolved with the anthocyanin by centrifugation, a crude extract is obtained after decompression and concentration, the crude extract is filtered, adsorbed, eluted and collected, the anthocyanin is obtained after concentration and drying, and an integrated red raspberries anthocyanin extraction device is adopted, so that the extraction rate is improved, and the labor cost is reduced.)

1. A method for extracting anthocyanin from red raspberries is characterized by comprising the following steps: comprises the following steps

S1, taking cleaned and impurity-removed red raspberries as raw materials, crushing and pulping in a food processor, mixing red raspberries pulp with an extracting agent according to the mass-volume ratio of 1: 10-1: 15, and ultrasonically extracting for 25min in a 400W ultrasonic extractor at the temperature of 30 ℃ to obtain an extraction mixed solution A;

s2, extracting the mixed liquor A, and centrifuging for 20min in a centrifugal machine (3) at 8000r/min to obtain a precipitate and a clear liquid B;

s3, taking the clear liquid B, and performing filter pressing by using a plate and frame filter press to obtain a filtrate C;

s4, placing the filtrate C at the temperature of 60 ℃ and concentrating under reduced pressure to obtain anthocyanin crude extract D;

s5, enabling the anthocyanin crude extract D to pass through an adsorption column (5) filled with XAD-7 macroporous resin at the flow rate of 2-3 times of column volume/h, enabling the anthocyanin to be adsorbed and saturated by the macroporous resin, then eluting the anthocyanin adsorbed by the macroporous resin with 80% ethanol solution at the flow rate of 2-3 times of column volume/h, and collecting eluent E;

s6, placing the eluent E at the temperature of 60 ℃ and carrying out reduced pressure concentration to obtain an anthocyanin concentrated solution F;

s7, placing the anthocyanin concentrated solution F at the temperature of-42 ℃ for vacuum freeze drying to obtain the raspberry anthocyanin;

the anthocyanin extraction process is realized by adopting integrated anthocyanin extraction equipment.

2. The extraction method of the anthocyanin of the red raspberry according to claim 1, wherein the extraction method comprises the following steps: the extractant is a methanol solution with the volume fraction of 80%.

3. An integral type anthocyanin extraction equipment, includes beating machine (1), its characterized in that: beating machine (1) bottom is connected with the ultrasonic extraction ware, and the ultrasonic extraction ware passes through valve (2) with the appearance chamber one side of centrifuge (3) and is connected, and the appearance chamber opposite side of centrifuge (3) passes through valve (2) and is connected with concentrated chamber (4), separate for two sliding chamber (41) by baffle (47) in concentrated chamber (4), sliding chamber (41) sliding connection has piston (46), two adsorption column (5) intercommunication through concentrated chamber (4) side sliding chamber (41), adsorption column (5) intussuseption is filled with macroporous resin, sliding chamber (41) side is connected with the solution tank through the liquid pipe, sliding chamber (41) are connected with vacuum drying case (6) through valve (2).

4. The integrated anthocyanin extraction device of claim 3, wherein: the side wall of the concentration cavity (4) is of a hollow structure, the inner wall (43) of the concentration cavity (4) is metal, the outer side of the inner wall (43) of the concentration cavity (4) is fixedly connected with a spirally wound heating wire, and vacuum is formed between the inner wall (43) and the outer wall (42).

5. The integrated anthocyanin extraction device of claim 4, wherein: the concentrating cavity (4) is cylindrical, the partition plate (47) is fixed in the middle of the concentrating cavity (4), and the side face of the piston (46) is attached to the side face of the sliding cavity (41).

6. The integrated anthocyanin extraction device of claim 3, wherein: centrifuge (3) hold intracavity sliding connection have filter-pressing board (33), filter-pressing board (33) top is connected with actuating lever (335) that are fixed in cylinder (45) that hold the chamber top, filter-pressing board (33) include with actuating lever (335) fixedly connected with foraminiferous clamp plate (331) of cylinder (45), it has the resistance plate to rotate on foraminiferous clamp plate (331).

7. The integrated anthocyanin extraction device of claim 6, wherein: the perforated pressure plate (331) is provided with filtering holes (3311) which are linearly arrayed along the diameter direction of the perforated pressure plate, the baffle plate comprises a rotating ring (332) which is rotationally connected with a driving rod (335) of the air cylinder (45), sealing plates (333) which are attached to the perforated pressure plate (331) and are annularly arrayed with the center of the rotating ring (332) are fixed on the rotating ring (332), and the number of the sealing plates (333) corresponds to the number of rows of the filtering holes (3311).

8. The integrated anthocyanin extraction device of claim 7, wherein: the rotating ring (332) is connected with a spring (334) sleeved on the driving rod (335), and the other end of the spring (334) is fixedly connected with the air cylinder (45).

Technical Field

The invention relates to the field of anthocyanin extraction, and particularly relates to a method for extracting red raspberry anthocyanin.

Background

The anthocyanin has the functions of resisting oxidation, scavenging free radicals and resisting mutation, and is widely applied to food production as a natural additive, and the red raspberry anthocyanin is the anthocyanin extracted from the red raspberry and has higher nutritional value.

Application document CN108003128B discloses a method for extracting grape seed procyanidin. The invention overcomes the problems that the procyanidine in the grape seed peel is difficult to dissolve out and the procyanidine in the extract has high polymerization degree, aspergillus niger is adopted as a strain to ferment grape seeds, enzymes such as cellulase, pectinase and the like generated by the aspergillus niger are utilized to degrade the grape seed peel so as to be beneficial to dissolving out the procyanidine, ethanol with different volume fractions is adopted as desorption liquid to elute macroporous adsorption resin, the procyanidine is graded, and then partial acidolysis is carried out so as to be beneficial to increasing the content of procyanidine oligomers in the extract. The content of oligomeric proanthocyanidins in the extract obtained by the invention is more than or equal to 98%, the average polymerization degree of the oligomeric proanthocyanidins is 2.5-3.0, the oligomeric proanthocyanidins can be easily absorbed in vivo, and the antioxidant activity is strong.

However, the prior art has low efficiency of extracting anthocyanin through multiple steps, and cannot meet the use requirement.

Disclosure of Invention

The invention aims to provide an extraction method of red raspberry anthocyanin, and aims to solve the technical problem of low extraction efficiency of anthocyanin.

In order to achieve the purpose, the invention provides the following technical scheme:

a method for extracting anthocyanin from red raspberry comprises the following steps

S1, taking cleaned and impurity-removed red raspberries as raw materials, crushing and pulping in a pulping machine, mixing red raspberries pulp with an extracting agent according to the mass-volume ratio of 1: 10-1: 15, and ultrasonically extracting for 25min in a 400W ultrasonic extractor at the temperature of 30 ℃ to obtain an extraction mixed solution A;

s2, extracting the mixed liquor A, and centrifuging for 20min in a centrifugal machine at 8000r/min to obtain a precipitate and a clear liquid B;

s3, taking the clear liquid B, and performing filter pressing by using a plate and frame filter press to obtain a filtrate C;

s4, placing the filtrate C at the temperature of 60 ℃ and concentrating under reduced pressure to obtain anthocyanin crude extract D;

s5, enabling the anthocyanin crude extract D to pass through an adsorption column filled with XAD-7 macroporous resin at the flow rate of 2-3 times of column volume/h, enabling the anthocyanin to be adsorbed and saturated by the macroporous resin, then eluting the anthocyanin adsorbed by the macroporous resin with 80% ethanol solution at the flow rate of 2-3 times of column volume/h, and collecting eluent E;

s6, placing the eluent E at the temperature of 60 ℃ and carrying out reduced pressure concentration to obtain an anthocyanin concentrated solution F;

s7, placing the anthocyanin concentrated solution F at the temperature of-42 ℃ for vacuum freeze drying to obtain the raspberry anthocyanin;

the preparation process is realized by adopting integrated anthocyanin preparation equipment.

Preferably, the extractant is a methanol solution with a volume fraction of 80%.

The utility model provides a red raspberry anthocyanin's extraction equipment, includes the beating machine, the beating machine bottom connection has the ultrasonic wave extractor, and the ultrasonic wave extractor passes through the valve with centrifuge's appearance chamber one side and is connected, and centrifuge's appearance chamber opposite side passes through the valve and is connected with concentrated chamber, concentrated intracavity is separated by the baffle for two sliding chambers, and sliding chamber sliding connection has a piston, two sliding chamber passes through the adsorption column intercommunication of concentrated chamber side, the adsorption column intussuseption is filled with macroporous resin, the sliding chamber side is passed through the liquid pipe and is connected with the solution tank, the sliding chamber passes through the valve and is connected with vacuum drying case.

Preferably, the side wall of the concentration cavity is of a hollow structure, the inner wall of the concentration cavity is made of metal, the outer side of the inner wall of the concentration cavity is fixedly connected with a heating wire which is spirally wound, and vacuum is formed between the inner wall and the outer wall.

Preferably, the concentration cavity is cylindrical, the partition plate is fixed in the middle of the concentration cavity, and the side surface of the piston is attached to the side surface of the sliding cavity.

Preferably, the centrifuge holds the intracavity sliding connection and has the filter-pressing board, the filter-pressing board top is connected with the actuating lever that is fixed in the cylinder that holds the chamber top, the filter-pressing board include with the actuating lever fixedly connected with foraminiferous clamp plate of cylinder, rotate on the foraminiferous clamp plate and be connected with the resistance plate.

Preferably, the perforated pressure plate is provided with filtering holes in a linear array along the diameter direction of the perforated pressure plate, the resistance plate comprises a rotating ring which is rotatably connected with a driving rod of the air cylinder, sealing plates which are attached to the perforated pressure plate and are in an annular array with the center of the rotating ring are fixed on the rotating ring, and the number of the sealing plates corresponds to the number of rows of the filtering holes.

Preferably, the swivel is connected with a spring sleeved on the driving rod, and the other end of the spring is fixedly connected with the cylinder.

Compared with the prior art, the invention has the beneficial effects that:

1. the method comprises the following steps of crushing cell walls of the red raspberries by a beater and an ultrasonic extractor, exposing anthocyanin in the cell walls and the cell walls to an organic solvent, centrifuging to separate the cell walls and other substances in the cell from a solution dissolved with the anthocyanin, carrying out decompression compression to obtain a crude extract, filtering, adsorbing, eluting, collecting, concentrating and drying to obtain the anthocyanin, and adopting integrated red raspberries anthocyanin extraction equipment to improve extraction rate and reduce labor cost.

2. In the integrated extraction equipment, a concentration cavity is divided into two sliding cavities by adopting a partition plate, the sliding cavities are communicated through an adsorption column and connected with a piston, and a solution in one sliding cavity is adsorbed through the adsorption column in a pressurizing mode, so that the crude extract can be repeatedly adsorbed and eluted, and the extraction rate of anthocyanin in the crude extract is ensured;

3. the filter pressing plate is connected in the accommodating cavity of the centrifuge in a sliding mode, the spring is connected with the rotating ring on the sealing plate, after the pressure reaches a certain degree, the sealing plate can rotate to block the filter hole under the action of the tensile force of the spring, and supernatant is obtained through direct filter pressing.

Drawings

FIG. 1 shows an integrated anthocyanin extraction apparatus of the present invention;

FIG. 2 is a cross-sectional view of a concentrating chamber of the present invention;

FIG. 3 is a cross-sectional view of the chamber of the centrifuge of the present invention;

FIG. 4 is a schematic structural view of a filter press plate according to the present invention

In the figure 1, a beater; 2. a valve; 3. a centrifuge; 31. a lower cavity; 32. an upper cavity; 33. pressing the filter plate; 331. a pressing plate with holes; 3311. filtering holes; 3312. a stop lever; 332. rotating the ring; 333. a sealing plate; 334. a spring; 335. a drive rod; 34. sealing the rotary sleeve; 4. a concentration chamber; 41. a slide chamber; 42. an outer wall; 43. an inner wall; 44. an electric heating wire; 45. a cylinder; 46. a piston; 47. a partition plate; 5. an adsorption column; 6. and (5) drying in a vacuum drying oven.

Detailed Description

Example 1

A method for extracting anthocyanin from red raspberries comprises the following steps:

cleaning 2kg of red raspberry with clear water, adding the cleaned red raspberry into a beater 1, fully crushing the red raspberry to form raw material pulp, mixing the red raspberry pulp and a methanol solution according to the mass-to-volume ratio of 1: 12.5, carrying out ultrasonic extraction for 25min in an ultrasonic extractor under the conditions of the temperature of 30 ℃ and 400W, and extracting a mixed solution A of the red raspberry with fully crushed cell walls and the methanol; centrifuging the mixed solution A in a centrifuge 3 at 8000r/min for 20min to obtain precipitate and clear solution B, wherein the clear solution B is the solution formed by mixing anthocyanin soluble in organic solvent in red raspberry and organic solvent, and removing the precipitate; carrying out filter pressing on the clear liquid B to obtain filtrate C;

concentrating the filtrate C under reduced pressure at 60 deg.C to obtain crude anthocyanin extractive solution D; enabling the anthocyanin crude extract D to pass through an adsorption column 5 filled with XAD-7 macroporous resin at the flow rate of 2-3 times of column volume/h, enabling the anthocyanin to be adsorbed and saturated by the macroporous resin, then eluting the anthocyanin adsorbed by the macroporous resin with 80% ethanol solution at the flow rate of 2-3 times of column volume/h, and collecting eluent E; concentrating the eluate E at 60 deg.C under reduced pressure to obtain anthocyanin concentrate F; and (3) placing the anthocyanin concentrated solution F at the temperature of-42 ℃ for vacuum freeze drying to obtain the red raspberry anthocyanin, and extracting by adopting integrated anthocyanin extraction equipment in the process, wherein the effective extraction rate is over 95 percent, and the extraction efficiency is high.

Example 2

As shown in fig. 1-4, the washed raspberry is added into a beater 1, the raspberry is pulped by a crushing shaft rotating in the beater 1, methanol is added into the beater 1 in a way of adopting the existing adding mechanism to be communicated with the top end of the beater 1, the adding mechanism is used as a solvent for washing the beater 1 on one hand and the raspberry on the other hand, then a valve 2 between the beater 1 and an ultrasonic extractor is opened, since the ultrasonic extractor is a prior art extractor, not shown in fig. 1, it should be connected between the beater 1 and the centrifuge 3, performing ultrasonic treatment for 25min at 30 deg.C and 400W to ensure cell wall complete breakage, opening valve 2 between ultrasonic extractor and centrifuge 3, centrifuging the solution in centrifuge 3 for 20min, and opening valve 2 to allow the centrifuged supernatant to enter concentration chamber 4.

The side wall of the concentration cavity 4 is arranged in a vacuum mode between the outer wall 42 and the inner wall 43, heat dissipation and overflow in the concentration process can be reduced, the concentration efficiency is improved, the energy consumption is reduced, the electric heating wire 44 fixed on the outer side of the inner wall 43 supplies heat to the inner wall 43 made of metal after the circuit is conducted, the inner part of the inner wall 43 is heated to 60 ℃ and then is subjected to heat preservation and concentration, the inner part of the concentration cavity 4 is divided into two parts by the partition plate 47, the first concentration is carried out in the sliding cavity 41 on one side of the partition plate 47, after the concentration is finished, the piston 46 is driven to move downwards by controlling the air cylinder 45 connected with the piston 46 in the sliding cavity 41, the inner part of the sliding cavity 41 is pressurized, under the action of certain pressure, the concentrated solution in the sliding cavity 41 passes through the adsorption column 5 at a certain flow rate, a large hole filled in the adsorption column 5 is vertically used for adsorbing anthocyanin, and the concentrated solution after the adsorption enters the sliding cavity 41 on the other side of the partition plate 47, then the piston 46 is driven by the cylinder 45 to move to increase the internal pressure of the sliding cavity 41 filled with the concentrated solution, the concentrated solution moves reversely again, the anthocyanin which is not completely adsorbed in the concentrated solution is secondarily adsorbed by the perforated resin again, then the concentrated solution which repeatedly passes through the adsorption column 5 is discharged, 80% ethanol solution is added into one of the chutes, the anthocyanin which is adsorbed in the macroporous resin is eluted by passing through the adsorption column 5 under certain pressure under the drive of the cylinder 45, the eluent can be repeatedly washed to improve the elution rate, the eluent adopts 80% ethanol solution, the adding mode can adopt the mode that the side surface of the concentrating cavity 4 is connected with equipment which adds solvent in the prior art, after the anthocyanin is heated and concentrated again, the valve 2 between the concentrating cavity 4 and the vacuum drying box 6 is opened, so that the concentrated eluent enters the vacuum drying box 6 to be dried to obtain the anthocyanin, can accomplish concentrated process repeatedly in concentrated chamber 4, and can adsorb, elute repeatedly, improve the effective extraction rate of anthocyanin, it needs to understand that beating machine 1, supersound extractor, centrifuge 3, concentrated chamber 4 heating wire 44 and cylinder 45, vacuum drying cabinet 6, valve 2 still need corresponding drive arrangement and controlgear control its operation, its controller adopts current PLC controller.

Example 3

As shown in fig. 1-4, when the solution centrifuged by the centrifuge 3 is used to extract the supernatant, the driving rod 335 slidably connected to the top of the chamber drives the filter press plate 33 to move downward, at this time, the filter holes 3311 of the perforated press plate 331 in the filter press plate 33 are staggered from the sealing plate 333 rotatably connected to the driving rod 335 through the rotary ring 332, the supernatant is squeezed above the filter press plate 33 through the filter holes 3311, when the driving rod 335 moves downward to contact with the precipitate, because the bottom end of the spring 334 is connected to the rotary ring 332 in a non-perpendicular manner, part of the pulling force of the spring 334 on the rotary ring 332 is converted into a transverse force on the rotary ring 332 to rotate the rotary ring 332 relative to the driving rod 335, until the sealing plate 333 fixedly connected to the rotary ring 332 abuts against the stop rod 3312 on the perforated press plate 331, the sealing plate 333 completely seals the filter holes 3311 to separate the precipitate from the supernatant, at this time, the valve 2 is opened to allow the supernatant to flow into the concentration chamber 4, in order to ensure that the supernatant can completely flow out, the height of the discharge port can be set to be a fixed value, and in the case that the raw material and the additive solution are fixed values, the precipitation amount should be also set to be a fixed height.

The chamber is arranged to be connected in a discontinuous mode with the upper chamber 32 and the lower chamber 31, the upper chamber 32 and the lower chamber 31 are connected through the sealing rotating sleeve 34, when the motor drives the lower chamber 31 to rotate, the solution in the lower chamber 31 rotates along with the rotation and completes the centrifugation, and meanwhile, the upper chamber 32 and the driving rod 335 and the valve 2 connected with the upper chamber are fixed on the premise of sealing, so that the centrifugal effect is prevented from being influenced by the unstable gravity center in the centrifugation process due to the rotation of the upper chamber.