CN214528799U - Special chromatographic device for preparing high-purity black rice anthocyanin by secondary column chromatography - Google Patents
Special chromatographic device for preparing high-purity black rice anthocyanin by secondary column chromatography Download PDFInfo
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- CN214528799U CN214528799U CN202120486006.XU CN202120486006U CN214528799U CN 214528799 U CN214528799 U CN 214528799U CN 202120486006 U CN202120486006 U CN 202120486006U CN 214528799 U CN214528799 U CN 214528799U
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Abstract
The utility model discloses a special chromatographic device for preparing high-purity black rice anthocyanin by secondary column chromatography, which comprises a constant-pressure water supply system, a feed liquid storage tank and a chromatographic column device, wherein a feed inlet of the constant-pressure water supply system is communicated with the feed liquid storage tank, and a second interface of the chromatographic column device is communicated with a liquid discharge pipe through a fifth valve, a third pipeline and a sixth valve; the first pipeline, the first valve, the first interface, the chromatographic column device, the third interface, the fourth valve and the liquid discharge pipe form an adsorption and desorption loop; the first pipeline, the second valve, the second pipeline, the third valve, the third interface, the chromatographic column device, the second interface, the fifth valve, the third pipeline, the sixth valve and the liquid discharge pipe form a back washing loop. The utility model discloses can realize further purifying and refining ordinary commercially available low-purity black rice extract product that anthocyanidin content is 10-25% obtain the high-purity black rice anthocyanin of anthocyanidin content 30-60%.
Description
Technical Field
The utility model relates to a chromatography device for preparing high-purity black rice anthocyanin by secondary column chromatography, which belongs to the technical field of natural plant extraction.
Background
The black rice is a special variety formed by long-term cultivation of gramineous plant rice, is a treasure in rice, is vegetatively reputed as tribute rice, medicinal rice and longevity rice, and has special nutritional value. The black rice has high nutritive value and medicinal value, and is recorded in compendium of materia medica: has effects in nourishing yin, invigorating kidney, invigorating spleen, warming liver, improving eyesight, and promoting blood circulation. It has excellent curative effect on dizziness, anemia, leukotrichia, eye diseases, etc.
The color of black rice is different from that of other rice mainly because the outer skin layer contains natural plant pigment, namely anthocyanin, which has strong anti-aging effect. The total flavone substance in the black rice peel mainly comprises black rice anthocyanin.
The anthocyanin is a water-soluble natural pigment widely existing in plants in the nature, is also a main coloring matter in plant petals, is related to most of colorful colors of fruits, vegetables, flowers and the like, is widely existing in plants such as black rice, blueberries, bilberry, purple cabbage and the like, is a pure natural edible pigment with certain nutrition and pharmacological effects, and can resist various related diseases caused by free radicals of a human body. The health preserving and health care efficacy of anthocyanins is well known internationally and is known as "soft gold". In the beauty treatment world in western countries such as europe and the united states, anthocyanins are called "youth nutrition" and "oral cosmetics", and have been widely used for their antioxidant and radical-scavenging effects.
The black rice contains a large amount of anthocyanin, the marked component of the black rice extract is black rice anthocyanin, the content of the anthocyanin in the black rice extract produced in the domestic production and manufacturing industry is generally 10-25%, individual manufacturers can achieve the purity of the black rice anthocyanin close to 30%, the extraction method of the black rice extract has water extraction, alcohol extraction, enzymolysis, supercritical method and the like, but the purification and refining method is mainly based on macroporous resin column chromatography purification basically, when the black rice extract is used as a health-care functional food raw material or is added and used in the fields of medicines and cosmetics, the purity of the anthocyanin is important, the purity of the anthocyanin raw material used in the fields of foods and medicines in developed countries in Europe and America is generally more than 35%, and therefore, the preparation method of the high-purity black rice anthocyanin suitable for large-scale production has practicability and practical guiding significance. The application prospect of the high-purity black rice anthocyanin in the fields of health food, medicine and export trade of natural plant extracts is expected to be extremely wide.
Disclosure of Invention
The utility model aims at providing a special chromatographic device of high-purity black rice anthocyanin is prepared to secondary column chromatography. The utility model takes the common commercially available black rice extract (the anthocyanin content is 10-25%) as the raw material, and prepares the high-purity black rice anthocyanin dry powder through polyamide column chromatography purification, desorption solution concentration and spray drying.
The process for preparing the high-purity black rice anthocyanin by the secondary column chromatography comprises the following steps:
1. column loading liquid pretreatment: according to the weight portion, the anthocyanin content of the commercially available black rice extract raw material is 10-25%, 10-15 portions of the commercially available black rice extract raw material are weighed, 100 portions of hydrochloric acid aqueous solution are fully stirred and dissolved at the temperature of 30-60 ℃, and the volume ratio concentration of the adopted hydrochloric acid aqueous solution is 2%.
2. Preparing a desorption solution: preparing an ethanol solution with the volume ratio of 60 percent, and adding 2 percent V/V hydrochloric acid.
3. The pressure of upper column liquid, washing liquid and desorption liquid is controlled to keep high and constant by adopting a chromatographic column device, and the high-pressure penetrating power is used for ensuring that feed liquid stably and smoothly penetrates through polyamide resin of the chromatographic column;
4. column loading and adsorption: and adsorbing the pretreated upper column liquid in the feed liquid storage tank 12 by polyamide resin in the chromatographic column 147 through an adsorption and desorption loop of the chromatographic column device, wherein the upper column pressure is set to be 5-7 kg, and the flow rate is controlled to be 2-2.5 column volumes per hour.
5. Washing with water: and after adsorption, washing the polyamide resin in the chromatographic column 147 with the washing liquid in the feed liquid storage tank 12 through an adsorption and desorption loop of the chromatographic column device, setting the upper column pressure to be 7-9 kg, controlling the flow rate to be 3-4 column volumes per hour, and washing until the eluent is clear.
6. Desorbing: after the water washing is finished, desorbing the polyamide resin in the chromatographic column 147 by using the desorption solution in the feed liquid storage tank 12 through an adsorption and desorption loop of a chromatographic column device, setting the column pressure of the desorption solution to be 5-7 kilograms, and controlling the flow rate to be 2.5-3 column volumes per hour to obtain the high-purity black rice anthocyanin desorption solution.
7. And (3) carrying out reduced pressure concentration, ethanol recovery and spray drying on the high-purity black rice anthocyanin desorption solution to obtain a dry powdery high-purity black rice anthocyanin finished product. The anthocyanin content of the high-purity black rice anthocyanin finished product is 30-60%.
8. Backwashing: the polyamide resin in the column 147 is backwashed by a backwash circuit of the column unit with alkaline and acidic backwash liquids alternately to restore the adsorption function of the polyamide resin.
A special chromatographic device for preparing high-purity black rice anthocyanin by secondary column chromatography comprises a constant-pressure water supply system, a feed liquid storage tank and a chromatographic column device, wherein a feed inlet of the constant-pressure water supply system is communicated with the feed liquid storage tank, an outlet of the constant-pressure water supply system is communicated with a first interface of the chromatographic column device through a first pipeline, a first valve is arranged between the first pipeline and the first interface, a third interface of the chromatographic column device is communicated with a liquid discharge pipe, the liquid discharge pipe is provided with a fourth valve, the first pipeline is communicated with the liquid discharge pipe at the inlet of the fourth valve through a second valve, a third valve and a second pipeline, and the second interface of the chromatographic column device is communicated with the liquid discharge pipe through a fifth valve, a third pipeline and a sixth valve;
the first pipeline, the first valve, the first interface, the chromatographic column device, the third interface, the fourth valve and the liquid discharge pipe form an adsorption and desorption loop;
the first pipeline, the second valve, the second pipeline, the third valve, the third interface, the chromatographic column device, the second interface, the fifth valve, the third pipeline, the sixth valve and the liquid discharge pipe form a back washing loop.
The chromatography column device comprises an enclosure, a first flange, a second flange, a baffle, a screen, a cylinder body, chromatography columns and end plates, wherein the end plates are arranged at two ends of the cylinder body, the peripheral surface of each end plate and the inner wall of the cylinder body are in a sealed state, a plurality of chromatography columns are tightly arranged in the cylinder body and penetrate through the end plates, the peripheral surface of each chromatography column and the hole wall of each end plate are in a sealed state, the first flange is welded at two ends of the cylinder body in a sealed mode, the second flange is welded at the enclosure at two ends of the cylinder body in a sealed mode, the first flange and the second flange are fixed together through bolts and nuts, the baffle and the screen are clamped between the first flange and the second flange, the screen is located on the inner side, and a plurality of through holes are formed in the baffle; a first connector and a second connector are arranged on the sealing cover on the upper part of the cylinder body; a third interface is arranged on the sealing cover at the lower part of the cylinder body; the chromatographic column is filled with 200-mesh polyamide resin by a wet method.
The diameter-height ratio of the chromatographic column is 1: 12.
the metal parts of the special chromatographic device are all made of stainless steel.
The utility model discloses a working process and principle:
the constant pressure water supply system keeps the pressure of the upper column liquid, the washing liquid and the desorption liquid high and constant, ensures that the feed liquid stably and smoothly permeates through the polyamide resin of the chromatographic column by using high-pressure penetrating power,
1. column loading and adsorption: the constant pressure water supply system absorbs the pretreated upper column liquid in the feed liquid storage tank through the polyamide resin in the chromatographic column through the adsorption and desorption loops of the chromatographic column device.
2. Washing with water: after the adsorption is finished, the constant-pressure water supply system washes the water washing liquid in the feed liquid storage tank through an adsorption and desorption loop of the chromatographic column device to wash the polyamide resin in the chromatographic column.
3. Desorbing: after the water washing is finished, the constant-pressure water supply system desorbs polyamide resin in the chromatographic column from the desorption solution in the feed liquid storage tank through an adsorption and desorption loop of the chromatographic column device, and the high-purity black rice anthocyanin desorption solution is obtained after desorption.
4. Backwashing: the polyamide resin in the column 147 is backwashed by a backwash circuit of the column unit with alkaline and acidic backwash liquids alternately to restore the adsorption function of the polyamide resin.
The utility model discloses use low-purity black rice extract as the raw materials, carry out secondary column chromatography purification through 200 mesh polyamide resin columns, utilize polyamide resin and anthocyanin molecule to pass through hydrogen bond and combine the selective adsorption principle, prepare high-purity black rice anthocyanin dry powder through desorption liquid concentration and spray drying again.
The beneficial effects of the utility model reside in that:
1. polyamide resin is the most ideal adsorbent for flavonoids, is mainly used for the subdivision and purification of flavonoids, and is different from the adsorption principle of macroporous resin, wherein the polyamide resin belongs to the chemical adsorption principle by virtue of hydrogen bond adsorption, the macroporous resin is the physical adsorption principle, and the finer the resin is in chromatographic application, the better the separation effect is. Therefore, the utility model discloses a 200 mesh polyamide resin secondary column chromatography separation purification black rice extract is the fundamental guarantee of preparation high-purity anthocyanin, can realize further purifying the refined high-purity black rice anthocyanin that obtains anthocyanin content 30-60% of the low-purity black rice extract of ordinary commercial anthocyanin content 10-25%.
2. The utility model discloses an application obstacle of polyamide resin in large-scale production is the velocity of flow problem that the resin fineness leads to, and resin fineness exceedes 60 mesh velocity of flow slows down, the permeability worsens in actual large-scale production, and resin fineness exceedes 100 meshes, and the normal pressure goes up the column velocity of flow and is close the stagnation, leads to the production cycle too long unable adaptation large-scale production manufacturing, so in actual production the producer mostly chooses macroporous resin purification to belong to nothing at all in fact, one of the novelty of the utility model is solved the application obstacle of more than 100 mesh polyamide resin in large-scale production, keeps high-order and invariable through adopting the pressure of chromatographic column device control upper column liquid, washing liquid, desorption liquid, guarantees with high pressure penetrating power that the feed liquid steadily smoothly permeates through polyamide resin, makes the velocity of flow controllable, and the permeability is good. The constant-pressure water supply system adopting the chromatographic column device adopts the prior art, and the control principle is that a high-pressure stainless steel pump is connected with the variable-frequency control of an intelligent constant-pressure control cabinet.
3. Polyamide resin is in column chromatography application, except that resin fineness subdivides the separation purification effect better more, and still a characteristic is that the big separation purification effect of footpath height ratio is better, generally footpath height ratio requires more than 1:8, and the laboratory can accomplish 1:50, but in actual large-scale production, is held the frame and operation platform high influence in the workshop, and the chromatographic column height adopts about 3 meters the price/performance ratio highest, the most convenient operation in the workman, one of the novelty of the utility model is practicality, the economic nature of guarantee large-scale production. Therefore, the chromatographic column adopts a combination mode that stainless steel is welded to manufacture small columns (the diameter-height ratio of the small columns is 1: 12) with the diameter of 0.2 meter and the height of 2.4 meters, and the small columns are assembled in a large column with the diameter of 1 meter or 0.6 meter in a bundling manner, 19 small columns can be assembled in the large column with the diameter of 1 meter, and 7 small columns can be assembled in the large column with the diameter of 0.6 meter. The advanced performance of the system is that the operation of a plurality of small chromatographic columns is met by one set of variable frequency pump feeding system of the intelligent constant-pressure control cabinet on the premise of ensuring the radial-height ratio, the space usage is saved, the labor is saved, and the auxiliary facilities are saved.
4. In the pretreatment of the upper column liquid, hydrochloric acid is added, because the anthocyanin has better solubility and stability in an acid solvent, the anthocyanin is heated to 30-60 ℃ for quick dissolution, and the anthocyanin is easy to be adsorbed by resin when being loaded on the column at high temperature.
5. In the preparation of the desorption solution, the purpose of adopting acid preparation is to facilitate desorption and ensure the stability of the anthocyanin.
Drawings
Fig. 1 is a schematic structural diagram of the present invention.
Figure 2 is a cross-sectional view of the chromatography column of the present invention.
Figure 3 is an end view of the chromatography column of the present invention.
Detailed Description
As shown in fig. 1, fig. 2 and fig. 3, a special chromatography device for preparing high-purity black rice anthocyanin by secondary column chromatography, the special chromatography device 1 comprises a constant-pressure water supply system 11, a feed liquid storage tank 12 and a chromatography column device 14, a feed inlet of the constant-pressure water supply system 11 is communicated with the feed liquid storage tank 12, an outlet of the constant-pressure water supply system 11 is communicated with a first interface 15 of the chromatography column device 14 through a first pipeline 13, a first valve 21 is arranged between the first pipeline 13 and the first interface 15, a third interface 17 of the chromatography column device 14 is communicated with a drain pipe 18, the drain pipe 18 is provided with a fourth valve 24, the first pipeline 13 is communicated with the drain pipe 18 at an inlet of the fourth valve 24 through a second valve 22, a third valve 23 and a second pipeline 19, and the second interface 16 of the chromatography column device 14 is communicated with the drain pipe 18 through a fifth valve 25, a third pipeline 20 and a sixth valve 26;
the first pipeline 13, the first valve 21, the first interface 15, the chromatographic column device 14, the third interface 17, the fourth valve 24 and the liquid discharge pipe 18 form an adsorption and desorption loop;
the first line 13, the second valve 22, the second line 19, the third valve 23, the third interface 17, the chromatography column device 14, the second interface 16, the fifth valve 25, the third line 20, the sixth valve 26 and the drain 18 constitute a back-flushing circuit.
The chromatographic column device 14 is composed of an enclosure 141, a first flange 142, a second flange 143, a baffle 144, a screen 145, a cylinder 146, chromatographic columns 147 and end plates 148, wherein the end plates 148 are arranged at two ends of the cylinder 146, the peripheral surface of the end plate 148 and the inner wall of the cylinder 146 are in a sealed state, the cylinder 146 is internally and tightly provided with the plurality of chromatographic columns 147, the plurality of chromatographic columns 147 penetrate through the end plates 148, the peripheral surface of each chromatographic column 147 and the hole wall of the end plate 148 are in a sealed state, the two ends of the cylinder 146 are hermetically welded with the first flange 142, the enclosure 141 at the two ends of the cylinder 146 is hermetically welded with the second flange 143, the first flange 142 and the second flange 143 are fixed together through bolts and nuts, the baffle 144 and the screen 145 are clamped between the first flange 142 and the second flange 143, the screen 14 is positioned at the inner side, and the baffle 144 is provided with a plurality of through holes 1441; the enclosure 141 on the upper part of the cylinder 146 is provided with a first interface 15 and a second interface 16; the enclosure 141 at the lower part of the cylinder 146 is provided with a third interface 17; the chromatographic column 147 is wet packed with 200 mesh polyamide resin.
The aspect ratio of the column 147 is 1: 12.
the metal parts of the special chromatographic device 1 are all made of stainless steel.
In this embodiment, the diameter of the chromatography column 147 is 0.2 m, the height of the chromatography column 147 is 2.4 m, the number of the chromatography columns 147 is 19, and the inner diameter of the cylinder 146 is 1 m; or the number of the chromatography columns 147 is 7, and the inner diameter of the cylinder 146 is 0.6 m.
The working process and principle of the special chromatographic device are as follows:
the constant pressure water supply system 11 keeps the pressure of the upper column liquid, the washing liquid and the desorption liquid high and constant, ensures that the feed liquid stably and smoothly permeates through the polyamide resin of the chromatographic column by using high-pressure penetrating power,
1. column loading and adsorption: the constant pressure water supply system 11 makes the pretreated upper column liquid in the feed liquid storage tank 12 pass through the adsorption and desorption loop of the chromatographic column device and be adsorbed by the polyamide resin in the chromatographic column 147.
2. Washing with water: after the adsorption is finished, the constant pressure water supply system 11 washes the polyamide resin in the chromatographic column 147 with the washing liquid in the feed liquid storage tank 12 through the adsorption and desorption loops of the chromatographic column device.
3. Desorbing: after the water washing is finished, the constant-pressure water supply system 11 desorbs the polyamide resin in the chromatographic column 147 from the desorption solution in the feed solution storage tank 12 through the adsorption and desorption loops of the chromatographic column device, and the high-purity black rice anthocyanin desorption solution is obtained after desorption.
4. Backwashing: the polyamide resin in the column 147 is backwashed by means of a backwash circuit of the column unit with alkaline and acidic backwash liquids to restore the adsorption function of the polyamide resin.
Claims (4)
1. The special chromatographic device for preparing the high-purity black rice anthocyanin by secondary column chromatography is characterized in that: the special chromatographic device (1) comprises a constant-pressure water supply system (11), a feed liquid storage tank (12) and a chromatographic device (14), wherein a feed inlet of the constant-pressure water supply system (11) is communicated with the feed liquid storage tank (12), an outlet of the constant-pressure water supply system (11) is communicated with a first interface (15) of the chromatographic device (14) through a first pipeline (13), a first valve (21) is arranged between the first pipeline (13) and the first interface (15), a third interface (17) of the chromatographic device (14) is communicated with a liquid discharge pipe (18), the liquid discharge pipe (18) is provided with a fourth valve (24), the first pipeline (13) is communicated with the liquid discharge pipe (18) at an inlet of the fourth valve (24) through a second valve (22), a third valve (23) and a second pipeline (19), the second interface (16) of the chromatography device (14) is communicated with the drain pipe (18) through a fifth valve (25), a third pipeline (20) and a sixth valve (26);
the first pipeline (13), the first valve (21), the first interface (15), the chromatography device (14), the third interface (17), the fourth valve (24) and the liquid discharge pipe (18) form an adsorption and desorption loop;
a first pipeline (13), a second valve (22), a second pipeline (19), a third valve (23), a third interface (17), a chromatography device (14), a second interface (16), a fifth valve (25), a third pipeline (20), a sixth valve (26) and a liquid discharge pipe (18) form a back washing loop;
the chromatography device (14) is composed of an enclosure (141), a first flange (142), a second flange (143), a baffle (144), a screen (145), a cylinder (146), chromatography columns (147) and end plates (148), wherein the end plates (148) are arranged at two ends of the cylinder (146), the peripheral surface of each end plate (148) is in a sealing state with the inner wall of the cylinder (146), a plurality of chromatography columns (147) are closely arranged in the cylinder (146), the plurality of chromatography columns (147) penetrate through the end plates (148), the peripheral surface of each chromatography column (147) is in a sealing state with the hole walls of the end plates (148), the first flange (142) is hermetically welded at two ends of the cylinder (146), the second flange (143) is hermetically welded at the enclosure (141) at two ends of the cylinder (146), the first flange (142) and the second flange (143) are fixed together through bolts and nuts, the baffle (144) and the screen (145) are clamped between the first flange (142) and the second flange (143), the screen is positioned at the inner side of the screen 14, and the baffle (144) is provided with a plurality of through holes (1441); the enclosure (141) at the upper part of the cylinder body (146) is provided with a first interface (15) and a second interface (16); the enclosure (141) at the lower part of the cylinder body (146) is provided with a third interface (17); the chromatographic column (147) is packed with 200 mesh polyamide resin by wet method.
2. The special chromatographic device for preparing the high-purity black rice anthocyanin by the secondary column chromatography in claim 1, is characterized in that: the diameter-height ratio of the chromatographic column (147) is 1: 12.
3. the special chromatographic device for preparing the high-purity black rice anthocyanin by the secondary column chromatography in claim 1, is characterized in that: the metal parts of the special chromatographic device (1) are all made of stainless steel.
4. The special chromatographic device for preparing the high-purity black rice anthocyanin by the secondary column chromatography in claim 2 is characterized in that: the diameter of the chromatographic column (147) is 0.2 m, the height of the chromatographic column (147) is 2.4 m, the number of the chromatographic columns (147) is 19, and the inner diameter of the cylinder body (146) is 1 m; or the diameter of the chromatographic column (147) is 0.2 m, the height of the chromatographic column (147) is 2.4 m, the number of the chromatographic columns (147) is 7, and the inner diameter of the cylinder body (146) is 0.6 m.
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| CN202120486006.XU CN214528799U (en) | 2021-03-08 | 2021-03-08 | Special chromatographic device for preparing high-purity black rice anthocyanin by secondary column chromatography |
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| CN202120486006.XU CN214528799U (en) | 2021-03-08 | 2021-03-08 | Special chromatographic device for preparing high-purity black rice anthocyanin by secondary column chromatography |
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