Application of a new hydrophilic-lipophilic balance resin microsphere in separation of fentanyl hydrolysate

Abstract

This invention discloses the application of a novel hydrophilic-lipophilic balanced resin microsphere in the separation of phytidine hydrolysates. The application includes the following steps: S1, loading a chromatography column with hydrophilic-lipophilic balanced resin microspheres wetted with water and / or alcohol, wherein the ratio of the column diameter to the column bed height is 1:1 to 1:20; S2, adding phytidine hydrolysate (with solid precipitate removed) to the chromatography column, wherein the sample volume to column bed volume ratio is 1:10 to 2:1, allowing the phytidine hydrolysate to flow into the column bed until the liquid level drops to the top of the column bed, then eluting with deionized water to obtain phosphate and inositol fractions; S3, concentrating and crystallizing the phosphate and inositol fractions respectively to obtain purified high-purity phosphate and inositol. This invention applies hydrophilic-lipophilic balanced resin microspheres to the separation of phytidine hydrolysates. This method does not employ ion exchange, does not generate large amounts of high-salt wastewater, is simple to operate, and is low in cost.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of separation and purification of phythin hydrolysate, and particularly relates to application of a novel hydrophilic-lipophilic balance resin microsphere in separation of phythin hydrolysate. BACKGROUND

[0002] Phythin is a complex salt of myo-inositol hexaphosphate (i.e. phytic acid) and metal ions such as calcium and magnesium. Phythin is widely present in the seeds of plants, such as wheat bran, rice bran, vegetables and the like. Phythin is mainly used for producing myo-inositol in industry. The process includes phythin hydrolysis, separation of main components myo-inositol and phosphate from the hydrolysate. The traditional separation method is that a part of phosphate is separated from the hydrolysate by crystallization, the hydrolysis reaction solution is sequentially subjected to cation and anion exchange resins, and the refining is repeatedly performed until the concentration of cations and anions in the hydrolysis reaction solution reaches a specified standard. The refined hydrolysis reaction solution is concentrated and crystallized to obtain the finished product myo-inositol. This method uses two kinds of ion exchange resins, and a large amount of high-salinity wastewater is generated in the production process, which needs to be solved urgently. SUMMARY

[0003] The application aims to provide application of a novel hydrophilic-lipophilic balance resin microsphere in separation of phythin hydrolysate. The application applies the hydrophilic-lipophilic balance resin microsphere to separation of phythin hydrolysate, and the separation method solves the problems of using two kinds of ion exchange resins and generating a large amount of high-salinity wastewater in the production process in the prior art, does not use the ion exchange mode, does not generate a large amount of high-salinity wastewater, is simple to operate, and is low in cost.

[0004] The application is implemented by the following technical scheme:

[0005] Application of a novel hydrophilic-lipophilic balance resin microsphere in separation of phythin hydrolysate, comprising the following steps:

[0006] S1, loading the hydrophilic-lipophilic balance resin microsphere soaked with water and / or alcohol into a chromatographic column, and the ratio of the column inner diameter to the column bed height of the chromatographic column is 1:1-1:20;

[0007] S2, adding the phythin hydrolysate from which the solid precipitate is removed into the chromatographic column, and the ratio of the sample volume to the column bed volume is 1:10-2:1, and after the phythin hydrolysate flows into the column bed, the liquid surface is lowered to be flush with the upper edge of the column bed, and deionized water is added for elution, to obtain phosphate and myo-inositol fractions respectively;

[0008] S3, concentrating and crystallizing the phosphate and myo-inositol fractions respectively to obtain refined high-purity phosphate and myo-inositol.

[0009] The specific steps of step S3 are: concentrating the phosphate stream to within 1 / 3 of the original stream volume, cooling and crystallizing to obtain refined high-purity phosphate or adding the concentrated phosphate solution into methanol to precipitate the phosphate; and concentrating the inositol stream to within 1 / 3 of the original volume, cooling and crystallizing to separate and obtain refined inositol.

[0010] Preferably, the particle size of the hydrophilic-lipophilic balance resin microspheres (HLB resin microspheres) in step S1 is 30-830 μm, the pore volume is 0.8-1.2 cm 3 / g, and the average pore size is

[0011] Preferably, the hydrophilic-lipophilic balance resin microspheres in step S1 are resin microspheres with the trade name HLB080 or HLB120 produced by MicroPure Biotech (Guangzhou) Co., Ltd.

[0012] Preferably, the hydrophilic-lipophilic balance resin microspheres in step S1 are immersed with water, and the ratio of the column inner diameter to the column bed height of the chromatographic column is 1:5.

[0013] Preferably, the hydrophilic-lipophilic balance resin microspheres in step S1 are immersed with a mixture of water and methanol or a mixture of water and ethanol, and then water is used to replace the column flow phase.

[0014] Preferably, in step S2, after the inositol stream flows into the column bed, the liquid level drops to the same level as the upper edge of the column bed, deionized water is added for elution, and the specific steps of obtaining the phosphate stream and the inositol stream are: after the inositol stream flows into the column bed, the liquid level drops to the same level as the upper edge of the column bed, deionized water is added for elution, the phosphate is eluted without reservation on the column, and the phosphate stream is obtained within 0.67-1.00 times the column bed volume of water. The elution is continued, and the inositol stream begins to flow out after 1-2 times the column bed volume of water is added. The column is renewed and activated after 2.5-4 times the column bed volume of water is added, and the inositol stream is obtained.

[0015] The application also protects a chromatographic column for separating and purifying inositol hydrolysate, wherein the ratio of the column inner diameter to the column bed height of the chromatographic column is 1:1-1:20, and the filler of the chromatographic column is hydrophilic-lipophilic balance resin microspheres immersed with water and / or alcohol. The hydrophilic-lipophilic balance resin microspheres are resin microspheres with the trade name HLB080 or HLB120 produced by MicroPure Biotech (Guangzhou) Co., Ltd.

[0016] Preferably, the particle size of the hydrophilic-lipophilic balance resin microspheres (HLB resin microspheres) is 30-830 μm, the pore volume is 0.8-1.2 cm 3 / g, and the average pore size is

[0017] Preferably, the chromatography column is made of glass, metal, or plastic.

[0018] Preferably, the ratio of the inner diameter of the chromatography column to the height of the column bed is 1:5.

[0019] Compared with the prior art, the beneficial effects of the present invention are: the present invention applies hydrophilic-lipophilic balanced resin microspheres to the separation of Fettin hydrolysate, the method does not use ion exchange mode, does not generate a large amount of high-salt wastewater, is simple to operate and low in cost. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of the chromatography column structure proposed in this invention. Detailed Implementation

[0021] The present invention will be further described in detail below with reference to the embodiments. These embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Experimental methods in the following embodiments that do not specify specific conditions are generally performed under conventional conditions in the art or as recommended by the manufacturer; the raw materials and reagents used, unless otherwise specified, are considered to be commercially available materials and reagents that can be obtained through conventional markets and other commercial channels.

[0022] like Figure 1 As shown, the chromatography column includes a column bed and a sieve plate disposed at the bottom of the column bed. The column bed is filled with packing material, preferably resin microspheres of brand HLB080 or HLB120 produced by Micropure Biotechnology (Guangzhou) Co., Ltd. In the following examples, either HLB080 or HLB120 can be selected as the HLB resin. In the following examples, the sodium or potassium salt of Fisting is added to a pressure hydrolysis vessel with water at a mass ratio of 1:2. The reaction is stirred at a hydrolysis pressure of 0.5-0.6 MPa for 8-10 hours. When the pH of the solution in the hydrolysis vessel is about 3-3.5, the hydrolysis is completed, and the hydrolysate is obtained.

[0023] Example 1

[0024] 30 g of HLB resin was packed into a 75 mL column with water. The column diameter was 3.2 cm and the column bed height was 18 cm. A 50 mL aqueous solution containing 4 g of inositol and 8 g of potassium dihydrogen phosphate was added to the column head. After all the aqueous solution had entered the column, pure water was added on top. Potassium dihydrogen phosphate was detected in the first 50 mL of eluent. After 150 mL of eluent, inositol was detected. After 250 mL of eluent, the column was completely regenerated. 7.6 g of potassium dihydrogen phosphate was recovered (95% recovery rate), and 3.8 g of inositol was recovered (95% recovery rate).

[0025] Example 2

[0026] 30 g of HLB resin was packed into a 75 mL column with water. The column diameter was 3.2 cm and the column bed height was 18 cm. 100 mL of aqueous solution containing 8 g of inositol and 16 g of potassium dihydrogen phosphate was added to the column head. After all the aqueous solution had entered the column, pure water was added on top. Potassium dihydrogen phosphate was detected in the first 50 mL of eluent. Inositol was detected in the eluent after 150 mL. The column was regenerated after 250 mL. 15.2 g of potassium dihydrogen phosphate was recovered (95% recovery rate), and 7.7 g of inositol was recovered (96% recovery rate).

[0027] Example 3

[0028] 30 g of HLB resin was packed with water into a 75 mL column with a diameter of 3.2 cm and a bed height of 18 cm. The sodium salt of Fisting was hydrolyzed, and the resulting hydrolysate was filtered and crystallized to separate sodium dihydrogen phosphate crystals. The mother liquor contained 12% inositol. The mother liquor was added to the HLB resin column at a sample volume to column bed volume ratio of 1:1, using water as the eluent. After one column bed volume, the sodium dihydrogen phosphate completely eluted. Further washing with 2.5 column bed volumes yielded inositol, which was then concentrated and crystallized, achieving a 95% recovery rate.

[0029] Example 4

[0030] 30 g of HLB resin was packed with water into a 75 mL column with a diameter of 3.2 cm and a bed height of 18 cm. The potassium salt of Fettin was hydrolyzed, and the resulting hydrolysate was filtered and crystallized to separate sodium dihydrogen phosphate crystals. The mother liquor contained 12% inositol. The mother liquor was added to the HLB resin column at a sample volume to column bed volume ratio of 1:1, using water as the eluent. After one column bed volume, the potassium dihydrogen phosphate completely eluted. Further washing with 2.5 column bed volumes yielded inositol. The inositol was then concentrated and crystallized, with a recovery rate of 95%.

[0031] Example 5

[0032] Similar to Example 1, except that the ratio of the column inner diameter to the column bed height was 1:1, and the ratio of the sample loading volume to the column bed volume was 1:10. 40 g of HLB resin was packed with water in a 100 mL column with a diameter of 5.1 cm and a bed height of 5.1 cm. The potassium salt of Fettin was hydrolyzed, and the resulting hydrolysate was filtered and crystallized to separate potassium dihydrogen phosphate crystals. The mother liquor contained 12% inositol. 10 mL of this solution was loaded, and after one column bed volume, the potassium dihydrogen phosphate completely eluted. After further washing with 3.0 column bed volumes, inositol was obtained. The inositol was then concentrated and crystallized, with a recovery rate of 96%.

[0033] Example 6

[0034] Similar to Example 1, except that the ratio of the column inner diameter to the column bed height was 1:20, and the ratio of the sample loading volume to the column bed volume was 2:1. 40 g of HLB resin was packed with water in a 100 mL column, with a column diameter of 1.85 cm and a column bed height of 37 cm. The potassium salt of Fettin was hydrolyzed, and the resulting hydrolysate was filtered and crystallized to separate potassium dihydrogen phosphate crystals. The mother liquor contained 12% inositol. 200 mL of this solution was loaded, and after one column bed volume, the potassium dihydrogen phosphate completely eluted. After further washing with 3.0 column bed volumes, inositol was obtained. The inositol was then concentrated and crystallized, with a recovery rate of 95%.

[0035] The above description of the embodiments is only for the purpose of helping to understand the technical solution and core idea of ​​the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made to the present invention without departing from the principle of the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.

Claims

1. The application of a novel hydrophilic-lipophilic balanced resin microsphere in the separation of phytidine hydrolysates, characterized in that, Includes the following steps: S1. A chromatography column is packed with hydrophilic-lipophilic balanced resin microspheres wetted with water and / or alcohol. The ratio of the column diameter to the column bed height is 1:1 to 1:

20. The particle size of the hydrophilic-lipophilic balanced resin microspheres is 30-830 μm, and the pore volume is 0.8-1.2 cm³. 3 / g, average pore size is S2. Add the phytidine hydrolysate (with solid precipitate removed) to the chromatography column. The ratio of sample volume to column bed volume is 1:10-2:

1. After the phytidine hydrolysate flows into the column bed and the liquid level drops to the top of the column bed, add deionized water for elution. Phosphate is not retained on the column. Elute completely within 0.67-1.00 times the column bed volume of water to obtain the phosphate fraction. Continue to add water for elution. After 1-2 times the column bed volume, the inositol-containing fraction begins to elute. After 2.5-4 times the column bed volume of water, the column is renewed and activated to obtain the inositol fraction. S3. The phosphate fraction is concentrated to less than 1 / 3 of the original fraction volume, cooled and crystallized to obtain refined high-purity phosphate, or the concentrated phosphate solution is added to methanol to precipitate phosphate; the inositol fraction is concentrated to less than 1 / 3 of the original inositol fraction volume, cooled and crystallized to obtain refined inositol.

2. The application according to claim 1, characterized in that, The hydrophilic-lipophilic balanced resin microspheres mentioned in step S1 are resin microspheres with the brand name HLB080 or HLB120 produced by Micropure Biotechnology (Guangzhou) Co., Ltd.

3. The application according to claim 1, characterized in that, In step S1, hydrophilic-lipophilic balanced resin microspheres that are wetted with water are packed into the chromatography column, and the ratio of the inner diameter of the chromatography column to the height of the column bed is 1:

5.

4. The application according to claim 1, characterized in that, In step S1, hydrophilic-lipophilic balanced resin microspheres wetted with a mixture of water and methanol or a mixture of water and ethanol are packed into the chromatography column, and then the mobile phase in the column is replaced with water.

5. A chromatography column for the separation and purification of phytidine hydrolysates, characterized in that, The ratio of the inner diameter of the chromatography column to the height of the column bed is 1:1 to 1:20, and the chromatography column packing material is hydrophilic-lipophilic balanced resin microspheres wetted with water and / or alcohol.

6. The chromatography column according to claim 5, characterized in that, The hydrophilic-lipophilic balanced resin microspheres have a particle size of 30-830 μm and a pore volume of 0.8-1.2 cm³. 3 / g, average pore size is 7. The chromatography column according to claim 5, characterized in that, The chromatography column materials include glass, metal, and plastic.

8. The chromatography column according to claim 5, characterized in that, The ratio of the inner diameter of the chromatography column to the height of the column bed is 1:5.

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