CN111001186A - Method for removing active carbon from ofloxacin eye drops - Google Patents
Method for removing active carbon from ofloxacin eye drops Download PDFInfo
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- CN111001186A CN111001186A CN202010012089.9A CN202010012089A CN111001186A CN 111001186 A CN111001186 A CN 111001186A CN 202010012089 A CN202010012089 A CN 202010012089A CN 111001186 A CN111001186 A CN 111001186A
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- active carbon
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/02—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor with moving adsorbents
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Abstract
The invention discloses a method for removing active carbon from ofloxacin eye drops, which comprises the following steps: step one, adding ofloxacin eye drops into a reaction bottle, then adding modified activated carbon, controlling the concentration of the modified activated carbon to be 0.02-0.04%, and then standing for 20-30min to obtain a blending solution. In the method for removing the active carbon from the ofloxacin eye drops, the decolorization rate and the impurity removal rate of the example 3 are both higher than 90 percent, while the decolorization rate and the impurity removal rate of the comparative example 1 are only 78.2 percent and 71.3 percent by removing the conventional active carbon; the modified active carbon and a proper treatment process can realize high efficiency of removing impurities and the like.
Description
Technical Field
The invention relates to the technical field of eye drops, in particular to a method for removing active carbon from ofloxacin eye drops.
Background
Ofloxacin is a quinolone broad-spectrum antibacterial drug, has strong antibacterial activity on gram-negative bacteria such as Escherichia coli, salmonella, Shigella and the like, and gram-positive bacteria such as staphylococcus aureus, streptococcus pneumoniae and the like, can be used for treating diseases such as urogenital system infection, respiratory tract infection, gastrointestinal tract infection and the like caused by sensitive bacteria, and can be prepared into eye drops for treating eye diseases such as blepharitis, dacryocystitis, hordeolum, conjunctivitis and the like.
Physical impurities and colors are doped in the production of ofloxacin eye drops, so that active carbon is required to be used for decoloring, the research on the adsorption of the active carbon in the prior art is not thorough, and how to realize an efficient adsorption method is the main research point of the invention.
Disclosure of Invention
The invention aims to provide a method for removing active carbon in ofloxacin eye drops so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the method for removing the active carbon from the ofloxacin eye drops comprises the following steps:
adding ofloxacin eye drops into a reaction bottle, adding modified activated carbon, controlling the concentration of the modified activated carbon to be 0.02-0.04%, and standing for 20-30min to obtain a blending solution;
step two, heating the blending liquid after standing in the step one, heating the temperature from room temperature to 70-75 ℃ at the speed of 2 ℃/min, and then carrying out heat preservation treatment;
step three, cooling the blending liquid subjected to heat preservation treatment in the step two, and reducing the cooling speed to room temperature at the speed of 5 ℃/min;
and step four, carrying out suction filtration and centrifugation on the blended solution recovered to the room temperature, and removing the active carbon.
Preferably, the modification method of the modified activated carbon comprises the following steps: soaking activated carbon in activating solution at 55-65 deg.C for 20-30min, and taking out60CorAnd (3) irradiating by using a radiation source, and then washing and drying to obtain the modified activated carbon.
Preferably, the activating solution comprises the following raw materials in parts by weight: 10-15 parts of citric acid, 2-5 parts of glutaric peroxide and 20-30 parts of water.
Preferably, the60CorThe total dose of radiation treatment by the radiation source is 4.5-5.5kGy, the radiation metering rate is 15.0-25.0Gy/min, and the radiation time is 10-20 min.
Preferably, the time of the heat preservation treatment in the second step is 10-20 min.
Preferably, the time of the heat preservation treatment in the second step is 15 min.
Preferably, the temperature is reduced to 40-45 ℃ before being cooled to the room temperature in the third step, the temperature is kept for 10-20min, and then the temperature is cooled to the room temperature.
Preferably, the temperature is reduced to 42.5 ℃ before being cooled to the room temperature in the third step, the temperature is kept for 15min, and then the temperature is cooled to the room temperature.
Compared with the prior art, the invention has the following beneficial effects:
in the method for removing the active carbon from the ofloxacin eye drops, the decolorization rate and the impurity removal rate of the example 3 are both higher than 90 percent, while the decolorization rate and the impurity removal rate of the comparative example 1 are only 78.2 percent and 71.3 percent by removing the conventional active carbon; the modified active carbon and a proper treatment process can realize high efficiency of removing impurities and the like.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the method for removing the active carbon from the ofloxacin eye drops comprises the following steps:
adding ofloxacin eye drops into a reaction bottle, adding modified activated carbon, controlling the concentration of the modified activated carbon to be 0.02%, and standing for 20min to obtain a blending solution;
step two, heating the blending liquid after standing in the step one, heating the temperature from room temperature to 70 ℃ at the speed of 2 ℃/min, and then carrying out heat preservation treatment;
step three, cooling the blending liquid subjected to heat preservation treatment in the step two, and reducing the cooling speed to room temperature at the speed of 5 ℃/min;
and step four, carrying out suction filtration and centrifugation on the blended solution recovered to the room temperature, and removing the active carbon.
Modification of the present exampleThe modification method of the charcoal comprises the following steps: soaking activated carbon in activating solution at 55 deg.C for 20-30min, and taking out60CorAnd (3) irradiating by using a radiation source, and then washing and drying to obtain the modified activated carbon.
The activating solution of the embodiment comprises the following raw materials in parts by weight: 10 parts of citric acid, 2 parts of glutaric acid peroxide and 20 parts of water.
Of the present embodiment60CorThe total dose of radiation treatment by the radiation source is 4.5kGy, the radiation metering rate is 15.0Gy/min, and the radiation time is 10 min.
The time for the heat preservation treatment in the second step of this embodiment is 10 min.
In the third step of this example, before cooling to room temperature, the temperature is first decreased to 40 ℃, the temperature is maintained for 10min, and then cooling to room temperature is performed.
Example 2:
the method for removing the active carbon from the ofloxacin eye drops comprises the following steps:
adding ofloxacin eye drops into a reaction bottle, adding modified activated carbon, controlling the concentration of the modified activated carbon to be 0.04%, and standing for 30min to obtain a blending solution;
step two, heating the blending liquid after standing in the step one, heating the temperature from room temperature to 75 ℃ at the speed of 2 ℃/min, and then carrying out heat preservation treatment;
step three, cooling the blending liquid subjected to heat preservation treatment in the step two, and reducing the cooling speed to room temperature at the speed of 5 ℃/min;
and step four, carrying out suction filtration and centrifugation on the blended solution recovered to the room temperature, and removing the active carbon.
The modification method of the modified activated carbon in the embodiment comprises the following steps: soaking activated carbon in activating solution at 65 deg.C for 30min, taking out60CorAnd (3) irradiating by using a radiation source, and then washing and drying to obtain the modified activated carbon.
The activating solution of the embodiment comprises the following raw materials in parts by weight: 15 parts of citric acid, 5 parts of glutaric acid peroxide and 30 parts of water.
Of the present embodiment60CorThe total dose of radiation treatment by the radiation source is 5.5kGy, the radiation metering rate is 25.0Gy/min, and the radiation time is 20 min.
The time for the heat preservation treatment in the second step of this embodiment is 20 min.
In the third step of this example, before cooling to room temperature, the temperature is first decreased to 45 ℃, and the temperature is maintained for 20min, and then cooled to room temperature.
Example 3:
the method for removing the active carbon from the ofloxacin eye drops comprises the following steps:
adding ofloxacin eye drops into a reaction bottle, adding modified activated carbon, controlling the concentration of the modified activated carbon to be 0.03%, and standing for 25min to obtain a blending solution;
step two, heating the blending liquid after standing in the step one, heating the blending liquid from room temperature to 72.5 ℃ at the speed of 2 ℃/min, and then carrying out heat preservation treatment;
step three, cooling the blending liquid subjected to heat preservation treatment in the step two, and reducing the cooling speed to room temperature at the speed of 5 ℃/min;
and step four, carrying out suction filtration and centrifugation on the blended solution recovered to the room temperature, and removing the active carbon.
The modification method of the modified activated carbon in the embodiment comprises the following steps: soaking activated carbon in activating solution at 60 deg.C for 25min, and taking out60CorAnd (3) irradiating by using a radiation source, and then washing and drying to obtain the modified activated carbon.
The activating solution of the embodiment comprises the following raw materials in parts by weight: 12.5 parts of citric acid, 3.5 parts of glutaric peroxide and 25 parts of water.
Of the present embodiment60CorThe total dose of radiation treatment by the radiation source is 5.0kGy, the radiation metering rate is 20.0Gy/min, and the radiation time is 15 min.
The time for the heat preservation treatment in the second step of this embodiment is 15 min.
In the third step of this example, the temperature is first decreased to 42.5 ℃ before cooling to room temperature, and the temperature is maintained for 15min, and then cooled to room temperature.
Comparative example 1.
The method is carried out by using conventional activated carbon.
The results of the performance tests of examples 1 to 3 and comparative example 1 are as follows
| Decolorization ratio (%) | Impurity removal Rate (%) | |
| Example 1 | 99.3 | 99.5 |
| Example 2 | 99.4 | 99.2 |
| Example 3 | 99.6 | 99.8 |
| Comparative example 1 | 78.2 | 71.3 |
From examples 1-3 and comparative example 1, the decolorization rate and impurity removal rate of example 3 of the invention are both as high as more than 90%, while the decolorization rate and impurity removal rate of comparative example 1 are only 78.2 and 71.3% by removing with conventional activated carbon.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. The method for removing the active carbon from the ofloxacin eye drops is characterized by comprising the following steps:
adding ofloxacin eye drops into a reaction bottle, adding modified activated carbon, controlling the concentration of the modified activated carbon to be 0.02-0.04%, and standing for 20-30min to obtain a blending solution;
step two, heating the blending liquid after standing in the step one, heating the temperature from room temperature to 70-75 ℃ at the speed of 2 ℃/min, and then carrying out heat preservation treatment;
step three, cooling the blending liquid subjected to heat preservation treatment in the step two, and reducing the cooling speed to room temperature at the speed of 5 ℃/min;
and step four, carrying out suction filtration and centrifugation on the blended solution recovered to the room temperature, and removing the active carbon.
2. The method for removing the active carbon from ofloxacin eye drops as claimed in claim 1, wherein the method for modifying the modified active carbon comprises: soaking activated carbon in activating solution at 55-65 deg.C for 20-30minAfter soaking, taking out60CorAnd (3) irradiating by using a radiation source, and then washing and drying to obtain the modified activated carbon.
3. The method for removing the active carbon in the ofloxacin eye drops according to claim 2, wherein the activating solution comprises the following raw materials in parts by weight: 10-15 parts of citric acid, 2-5 parts of glutaric peroxide and 20-30 parts of water.
4. The method of claim 2, wherein the step of removing the active carbon from the ofloxacin eye drops is carried out by a vacuum evaporation system60CorThe total dose of radiation treatment by the radiation source is 4.5-5.5kGy, the radiation metering rate is 15.0-25.0Gy/min, and the radiation time is 10-20 min.
5. The method for removing active carbon from ofloxacin eye drops as claimed in claim 1, wherein the time for the heat preservation treatment in step two is 10-20 min.
6. The method for removing active carbon from ofloxacin eye drops as claimed in claim 5, wherein the time for the heat preservation treatment in step two is 15 min.
7. The method for removing the active carbon from ofloxacin eye drops as claimed in claim 1, wherein the temperature is reduced to 40-45 ℃ before cooling to room temperature in step three, the temperature is kept for 10-20min, and then the temperature is cooled to room temperature.
8. The method for removing the active carbon from ofloxacin eye drops as claimed in claim 7, wherein the temperature is reduced to 42.5 ℃ in step III before cooling to room temperature, and the temperature is kept for 15min, and then cooled to room temperature.
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| CN109846820A (en) * | 2019-04-09 | 2019-06-07 | 广东三蓝药业股份有限公司 | A kind of ofloxacin eye drops and preparation method thereof |
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