Preparation process of vitamin E soft capsule

Abstract

The invention relates to a preparation process of a vitamin E soft capsule, which is characterized in that the process of blending, dissolving and pelleting is improved, and during blending, the ratio of vitamin E to corn oil is 1: 2, and the vitamin E and the corn oil are uniformly mixed in a common stirring and circulating stirring mode; the glue dissolving is also carried out under cyclic stirring, vacuumizing and defoaming are carried out after the glue dissolving, a hot glue solution is sieved by a 120-mesh sieve and transferred to a heat preservation glue barrel, and the heat preservation temperature of the heat preservation glue barrel is 60-70 DEG C; during pelleting, the temperature of a gelatin box is controlled to be 50-55 DEG C to be lower than the temperature of a heat preservation glue barrel and slightly higher than the temperature of a cloth spreading box, a glue solution is slowly stirred, the flow of the glue solution is accurately controlled through a flow valve, meanwhile, the temperature of a material injection spray head is controlled to be 35-50 DEG C, the rotating speed of a rolling die main shaft is controlled to be 2-6 r / min, and the rolling die pressure is controlled to be 0.2-0.3 MPa; according to the technology, the raw material characteristics and the forming technology are dynamically matched, through synchronous planning and linkage regulation and control, quality defects are fundamentally avoided, the product percent of pass is remarkably increased, and only about 1 kg of unqualified products with the vitamin E content of 48,000,000 are produced.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of biological medicine, and relates to the preparation of soft capsules, in particular to a preparation process of vitamin E soft capsules. BACKGROUND

[0002] The vitamin E soft capsule is a medicine prepared from vitamin E, corn oil, gelatin for capsules, glycerol, water and the like, and is one of the most important antioxidants. The vitamin E soft capsule has a wide range of effects, can promote the secretion of sex hormones, increase the activity and quantity of sperm in men, increase the concentration of female sex hormones in women, improve fertility, prevent miscarriage, and has good effects in preventing and treating male infertility, burns, frostbite, capillary bleeding, menopausal syndrome, beauty and the like. Vitamin E can also inhibit the peroxidation of lipids in the eye lens, dilate peripheral blood vessels, and improve blood circulation.

[0003] Although the existing vitamin E production process can ensure the preparation of qualified products, it still has some drawbacks, for example, the unqualified rate is high during the inspection of pills, and there are many irregular-shaped pills, thin-skinned pills and bubble pills, so the existing preparation process still needs to be further optimized. Although the applicant has been optimizing the preparation process of vitamin E, but the problem of high unqualified rate has not been solved, and attempts have been made to optimize the proportion of gelatin, glycerol and water, and adjust the sol temperature, but the effect is not ideal. SUMMARY

[0004] In view of the shortcomings and deficiencies of the prior art, the purpose of the present application is to provide a preparation process of vitamin E soft capsules, which significantly improves the product qualified rate by improving the process of preparation, sol and pill pressing, and produces only about 1 kg of unqualified product from 4.8 million particles (3815 kg of raw material), greatly improving the product qualified rate.

[0005] To achieve the above purpose, the technical scheme adopted by the present application is as follows:

[0006] A preparation process of vitamin E soft capsules, comprising the following steps:

[0007] Step 1. Preparation: Add vitamin E and corn oil into the ingredient tank, the proportion of the vitamin E and corn oil is 1:2, the inside of the ingredient tank is provided with a stirring mechanism, the outside is provided with a circulating passage in communication with the inside of the ingredient tank, a circulating pump is arranged on the circulating passage, and the stirring mechanism is stirred for 2-3 hours under water bath heating, then the circulating pump is circulated for 1-2 hours, then filtered and prepared for use;

[0008] Step 2. Sol: Add a certain amount of purified water to the gelatinizing tank, heat to 40-50℃, start the circulating pump on the circulating path between the outside of the gelatinizing tank and the inside of the gelatinizing tank, and add glycerol under circulating stirring until mixed, then continue to add gelatin powder, gradually heat to 70-80℃ under circulating stirring, and make the gelatin powder completely melt. The ratio of gelatin powder, purified water and glycerol during sol is 2:2:1, and the sol time is controlled within 60-70 minutes; then, stop the circulating stirring, vacuum degassing, control the vacuum degree in the gelatinizing tank < -0.07Mpa, and the vacuum time is 5-10 minutes; finally, the hot glue liquid is sieved through a 120 mesh sieve, transferred to a heat preservation glue barrel, the heat preservation temperature of the heat preservation glue barrel is 60-70℃, and the glue liquid is static for > 70 minutes before being used in the next step;

[0009] Step 3: pill pressing: the glue liquid in the heat preservation glue barrel is transported to the gelatin box through the pipeline, the temperature of the gelatin box is controlled at 50-55℃, a stirring mechanism is arranged in the gelatin box, the stirring speed is controlled at 5-20 revolutions per minute, a flow valve is arranged at the glue outlet, and the flow valve is used to match the pill pressing speed and the glue thickness, automatically adjusts according to the pill pressing speed and the glue thickness, and satisfies the formula: Q=(V / 2×N×k) / (1-η);

[0010] Wherein, Q is the volume flow of the glue liquid, unit: L / min; V is the glue liquid consumption of the glue shell of a single soft capsule, unit: L / capsule, V≈S×d; S is the surface area of the glue shell of a single soft capsule, unit: cm 2 ; d is the thickness of the glue, unit: cm; N is the pill pressing speed, unit: capsules / min; k is the correction coefficient, taken as 1.02-1.05, and η is the loss rate, η=(2V 胶皮 -V×n) / 2V 胶皮 , wherein V 胶皮 represents the glue liquid consumption of the glue with fixed size and thickness, and n represents the number of soft capsules prepared by using the glue with fixed size and thickness;

[0011] The glue liquid output from the gelatin box is transferred to the spreading box to prepare the glue skin, and the temperature of the spreading box is 40-50℃;

[0012] The prepared glue skin and the vitamin E prepared in step 1 are pressed into soft capsules by an automatic rotary capsule machine, the temperature of the injection nozzle is controlled at 35-50℃, the rotation speed of the roll mold main shaft is 2-6 revolutions per minute, and the roll mold pressure is 0.2-0.3MPa;

[0013] Finally, the soft capsule pills are transferred into the rotating cage, the rotation speed is set to 10-14 revolutions per minute, the air volume is 2500-3500m 3 , and the shaping time is 1-2h;

[0014] Step 4. Wipe dry: Place the 95% ethanol soaked clean cloth in the rotating basket, and wipe the soft capsule pellets with the clean cloth while the rotating basket is rotating, and then dry them;

[0015] Step 5. Check the pellets.

[0016] As a preferred embodiment of the present application, the temperature of the water bath heating in step 1 is controlled at 55℃±5℃, first stirred for 2.5 hours by the stirring mechanism, then stirred for 1 hour by the circulating pump, and then sieved through a 200 mesh sieve for standby.

[0017] As a preferred embodiment of the present application, the gelation tank in step 2 is a water bath type gelation tank.

[0018] As a preferred embodiment of the present application, after vacuumizing in step 2, the bubbles are detected, if there are still bubbles, the temperature is raised to 70-85℃ under the vacuum degree of <-0.07Mpa in the gelation tank, and the heating is stopped after 5-25 minutes to determine whether the defoaming is sufficient.

[0019] As a preferred embodiment of the present application, the clean cloth in step 4 is white, and the replacement frequency is 4 hours / time.

[0020] As a preferred embodiment of the present application, when drying in step 4, the temperature is set to 24-35℃, and the relative humidity is <40%, and the drying is ended when the soft capsules reach the standard of appropriate hardness and smoothness.

[0021] As a preferred embodiment of the present application, the flat pellets, large and small pellets, irregular shaped pellets, thin skin pellets and bubble pellets are picked out under the lamp inspection table in step 5.

[0022] The advantages and beneficial effects of the present application are:

[0023] (1) In the preparation process of the present application, ordinary stirring and circulating stirring are combined, the ratio of vitamin E and corn oil is reasonably controlled, the soft capsule content is uniformly mixed and has moderate viscosity, and the filling amount of each soft capsule content in the preparation process is ensured by reasonably controlling the temperature of the spray body, so as to avoid the appearance of large and small pellets, irregular shaped pellets or flat pellets due to inaccurate content filling amount.

[0024] (2) In order to balance the "production efficiency" and "molding quality", the present application not only ensures that each soft capsule can complete the whole process of "gel skin molding → content filling → compression sealing", but also meets the capacity demand of industrialized batch production, the main shaft speed is controlled at 2-6rpm, and the spray body temperature is controlled at 35-50℃. This design can ensure the smooth filling of the content and match the gel skin temperature on the premise of not damaging the effective ingredients, and ensure the sealing and molding quality of the soft capsules.

[0025] (3) the sol process and the pill pressing process can ensure that the prepared rubber skin has uniform thickness (about 0.8 mm), the rubber skin thickness error is ≤±0.05 mm, there is no bubble in the rubber skin, the forming quality is ensured, and large pills, flat pills, bubble pills or thin skin pills are avoided; in addition, a gelatin box is arranged between the heat preservation glue bucket and the spreading box, the temperature of the gelatin box is set to be lower than the temperature of the heat preservation glue bucket and slightly higher than the temperature of the spreading box, the glue solution is stirred in a slow stirring mode, and then the rubber skin is prepared; the step-by-step temperature control mode can further reduce the detection rate of bubble pills and ensure the quality of the prepared rubber skin.

[0026] (4) the raw material characteristics and the forming process are dynamically matched, the quality defects are fundamentally avoided through synchronous planning and linkage control, and the product quality is stabilized. Only about 1 kg of unqualified products is produced in the production process of the present application for 4.8 million vitamin E pills, and the product qualified rate is greatly improved. DETAILED DESCRIPTION

[0027] The application discloses a preparation process of vitamin E soft capsules. Those skilled in the art can refer to the content of the present application and appropriately improve the component parameters or process parameters. It should be particularly pointed out that all similar replacements and changes are obvious to those skilled in the art, and they are considered to be included in the protection scope of the present application.

[0028] Example 1

[0029] A preparation process of vitamin E soft capsules, the process comprising the following steps:

[0030] Step 1. Preparation: a dosing tank is added with vitamin E and corn oil, the ratio of the vitamin E to the corn oil is 1:2, the dosing tank is internally provided with a stirring mechanism, externally provided with a circulating passage in communication with the inside of the dosing tank, the circulating passage is provided with a circulating pump, and the vitamin E and the corn oil are stirred for 2-3 hours through the stirring mechanism under water bath heating, then stirred for 1-2 hours through the circulating pump, and then filtered and prepared.

[0031] Specifically, in the present embodiment, the water bath heating temperature is controlled at 55℃±5℃, the vitamin E and the corn oil are stirred for 2.5 hours through the stirring mechanism, then stirred for 1 hour through the circulating pump, and then prepared through a 200-mesh sieve.

[0032] Step 2. Sol: Add a certain amount of purified water to the water bath gel tank, heat to 40-50℃, start the circulating pump on the circulating path connected to the outside of the gel tank and the inside of the gel tank, and add glycerol under circulating stirring until mixed, then continue to add gelatin powder, gradually heat to 70-80℃ under circulating stirring, and the gelatin powder is completely melted. The ratio of gelatin powder, purified water and glycerol during sol is 2:2:1, and the sol time is controlled within 60-70 minutes; then, stop the circulating stirring, vacuum degassing, control the vacuum degree in the gel tank < -0.07Mpa, vacuum time 5-10 minutes, after vacuuming, detect the bubbles, if there are still bubbles, increase the temperature to 70-85℃ under the vacuum degree < -0.07Mpa in the gel tank, keep for 5-25 minutes, and stop heating after determining that the degassing is sufficient; finally, pass the hot glue solution through a 120 mesh sieve, transfer to a heat preservation glue barrel, the heat preservation temperature of the heat preservation glue barrel is 60-70℃, and the glue solution is static for > 70 minutes before being used in the next step;

[0033] Step 3: Press the pill: The glue solution in the heat preservation glue barrel is transported to the gelatin box through the pipeline, the temperature of the gelatin box is controlled at 50-55℃, a stirring mechanism is arranged in the gelatin box, the stirring speed is controlled at 5-20 revolutions per minute, a flow valve is arranged at the glue outlet, and the flow valve is used to match the pill pressing speed and the glue thickness, and automatically adjusts according to the pill pressing speed and the glue thickness, satisfying the formula: Q = (V / 2 x N x k) / (1-η);

[0034] Wherein, Q is the volume flow of the glue solution (unit: L / min); V is the glue solution consumption of the glue shell of a single soft capsule (unit: L / capsule), V≈S x d, S is the surface area of the glue shell of a single soft capsule (unit: cm 2 ), d is the thickness of the glue (unit: cm); N is the pill pressing speed (unit: particles / min); k is the correction coefficient, usually taken as 1.02-1.05, and η is the loss rate, which is determined according to the actual production data, η = (2V 胶皮 -V x n) / 2V 胶皮 , wherein V 胶皮 represents the glue solution consumption of the glue with fixed size and thickness, and n represents the number of soft capsules prepared by using the glue with fixed size and thickness;

[0035] The glue solution output from the gelatin box is transferred to the spreading box to prepare the glue skin, and the temperature of the spreading box is 40-50℃;

[0036] The prepared glue skin and the vitamin E prepared in step 1 are pressed into soft capsules by an automatic rotary capsule machine (also known as a full-automatic soft capsule machine), and the temperature of the injection nozzle (spray body) is controlled at 35-50℃, the rotating speed of the rolling die main shaft is 4 revolutions per minute, and the rolling die pressure is 0.25MPa;

[0037] Finally, the soft capsule pills are transferred into the rotating cage, the rotating speed is set to 10-14 rpm, and the air volume is 2500-3500 m 3 , the shaping time is 1-2 h;

[0038] Step 4. Wipe dry: Place clean cloths soaked in 95% ethanol in the rotating cage, and wipe the soft capsule pills with the clean cloths while the rotating cage is rotating, to ensure that the surface of the soft capsule pills is clean and free of excess oil, and then dry them;

[0039] Step 5. Check the pills: Under the lamp inspection table, pick out the flat pills, large and small pills, irregular pills, thin-skinned pills, and bubble pills.

[0040] In this embodiment, the clean cloths in step 4 are white, and 6 clean cloths are placed in each rotating cage, with a replacement frequency of 4 hours per time; when drying, the temperature is set to 24-35°C, and the relative humidity is <40%; when the soft capsules reach the appropriate hardness and smoothness standards, the drying is completed.

[0041] In this embodiment, the amounts of each raw material used to prepare 4.8 million vitamin E soft capsules are as follows: vitamin E: 480 kg; corn oil: 960 kg; gelatin for capsules: 950 kg; glycerol: 475 kg; purified water: 950 kg.

[0042] By weighing the unqualified pills detected, it is found that only about 1 kg of unqualified product is produced for 4.8 million vitamin E soft capsules, greatly improving the product qualification rate.

[0043] Comparative Example 1

[0044] The difference from Example 1 is that in step 1, the vitamin E and corn oil are mixed by ordinary stirring, and the ratio of vitamin E to corn oil is tried at 1:1.8 and 1:1.5. The results show that the detection rates of large and small pills, irregular pills, and flat pills are all increased.

[0045] Comparative Example 2

[0046] The difference from Example 1 is that in step 2, the sol is prepared by ordinary stirring (mechanical stirring), and the temperature of the heat preservation gel barrel is 45-60°C; in step 3, the gel solution in the heat preservation gel barrel is directly transferred to the gel skin preparation box through the gelatin box, the gelatin box is not provided with a stirring mechanism, and the flow rate is not strictly controlled. It is found that the thickness of the prepared gel skin is not uniform, the thickness is 0.6-0.9 mm, and the unqualified rate of the product is significantly increased, especially the number of thin-skinned pills, large and small pills, and irregular pills is significantly increased.

[0047] The above application of specific examples to the present application is described, only for help to understand the present application, and not to limit the present application. For the skilled in the art to which the present application belongs, according to the idea of the present application, several simple deductions, deformation or replacement can be made. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A process for the preparation of vitamin E soft gelatin capsules, characterized in that, The process comprises the following steps: Step 1. Preparation: add vitamin E and corn oil into a preparation tank, the ratio of vitamin E to corn oil being 1:2, the inside of the preparation tank being provided with a stirring mechanism, the outside of the preparation tank being provided with a circulating passage in communication with the inside of the preparation tank, the circulating passage being provided with a circulating pump, first stirring for 2-3 hours under water bath heating through the stirring mechanism, then circulating stirring for 1-2 hours through the circulating pump, then filtering, and reserving; Step 2. Sol: add a certain amount of purified water into a gelatinizing tank, heat to 40-50℃, start the circulating pump on the circulating passage outside the gelatinizing tank in communication with the inside of the gelatinizing tank, add glycerol until mixed under circulating stirring, then continue to add gelatin powder, gradually heat to 70-80℃ under circulating stirring, so that the gelatin powder is completely melted, the ratio of gelatin powder, purified water and glycerol being 2:2:1 during the sol process, the sol time being controlled within 60-70 minutes; then, stop the circulating stirring, vacuum degassing, control the vacuum degree in the gelatinizing tank to be less than -0.07Mpa, the vacuum time being 5-10 minutes; finally, pass the hot glue liquid through a 120-mesh sieve, transfer to a heat preservation glue barrel, the heat preservation temperature of the heat preservation glue barrel being 60-70℃, the glue liquid is stationary for more than 70 minutes before being used in the next step; Step 3: pill pressing: transfer the glue liquid in the heat preservation glue barrel to the gelatin box through the pipeline, control the temperature of the gelatin box to be 50-55℃, set a stirring mechanism in the gelatin box, control the stirring speed to be 5-20 revolutions per minute, set a flow valve at the glue outlet, the flow valve is used to match the pill pressing speed and the glue skin thickness, automatically adjust according to the pill pressing speed and the glue skin thickness, meet the formula: Q=(V / 2×N×k) / (1-η); Wherein, Q is the volume flow of the glue, unit: L / min; V is the glue consumption of the soft capsule shell, unit: L / piece, V≈Sxd; S is the surface area of the soft capsule shell, unit: cm 2 ; d is the thickness of the rubber, unit: cm; N is the speed of pressing the pill, unit: piece / min; k is the correction coefficient, taking 1.02-1.05, η is the loss rate, η=(2V 胶皮 -Vxn) / 2V 胶皮 , wherein V 胶皮 represents the glue consumption of the rubber with fixed size and thickness, and n represents the number of soft capsules prepared by using the rubber with fixed size and thickness. Transfer the glue liquid output by the gelatin box to the spreading box to prepare the glue skin, the temperature of the spreading box being 40-50℃; Prepare the glue skin and the vitamin E prepared in step 1 by the automatic rotary capsule machine, control the temperature of the injection nozzle to be 35-50℃, the rotating speed of the rolling die main shaft to be 2-6 revolutions per minute, the rolling die pressure to be 0.2-0.3MPa; Finally the soft capsule pill into the rotating cage, set the speed of 10-14 revolutions per minute, air volume of 2500-3500 m 3 , shaping time 1-2h; Step 4. Wipe and dry: place clean cloths soaked in 95% ethanol in a rotating cage, rotate the cage while wiping the soft capsules with clean cloths, then dry; Step 5. Check the pills.

2. The process for preparing vitamin E soft capsules according to claim 1, characterized in that, The temperature of the water bath heating in step 1 is controlled to be 55℃±5℃, first stirring for 2.5 hours through the stirring mechanism, then circulating stirring for 1 hour through the circulating pump, then passing through a 200-mesh sieve, and reserving.

3. The process for preparing vitamin E soft capsules according to claim 1, wherein, The gelatinizing tank in step 2 is a water bath type gelatinizing tank.

4. The process for preparing vitamin E soft capsules according to claim 1, wherein, After vacuumizing in step 2, detect the bubbles, if there are still bubbles, increase the temperature to 70-85℃ under the vacuum degree in the gelatinizing tank being less than -0.07Mpa, keep for 5-25 minutes, stop heating after determining that the degassing is sufficient.

5. The process for preparing vitamin E soft capsules according to claim 1, wherein the vitamin E is dissolved in the oil phase at a temperature of 60 to 80°C. The clean cloths in step 4 are white, and the replacement frequency is 4 hours per time.

6. The process for preparing vitamin E soft capsules according to claim 1, wherein, When drying in step 4, the temperature is set to be 24-35℃, the relative humidity is less than 40%, and the drying is completed when the soft capsules reach the standard of appropriate hardness and smoothness.

7. The process for preparing vitamin E soft capsules according to claim 1, wherein the vitamin E is dissolved in the oil phase by heating to 60-80°C. Pick out flat pills, large and small pills, irregular shaped pills, thin skin pills and bubble pills under the light inspection table in step 5.