CN107417563A - A kind of method that Doxycycline Hyclate is reclaimed in the refinement mother liquor from Doxycycline Hyclate - Google Patents
A kind of method that Doxycycline Hyclate is reclaimed in the refinement mother liquor from Doxycycline Hyclate Download PDFInfo
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- CN107417563A CN107417563A CN201710237660.5A CN201710237660A CN107417563A CN 107417563 A CN107417563 A CN 107417563A CN 201710237660 A CN201710237660 A CN 201710237660A CN 107417563 A CN107417563 A CN 107417563A
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Abstract
The invention discloses a kind of method that Doxycycline Hyclate is reclaimed in refinement mother liquor from Doxycycline Hyclate, including 1）Sulfosalicylic acid is added into Doxycycline Hyclate refinement mother liquor to be handled, is stood still for crystals, and is filtered to separating out solid A；2）Ethanol water is added to solid A is filtered out, mashing washing is carried out, filters out solid B；3）Solid B is added in ethanol water, ammoniacal liquor is added dropwise to solid dissolved clarification, is heated up after filtering, after crystallization, filters to obtain solid C；4）Solid C is added in ethanol water, hydrochloric acid, which is added dropwise, makes its dissolving, adds sulfosalicylic acid, after crystallization, is filtered to separating out solid D；5）Solid D is added in ethanol water, ammoniacal liquor is added dropwise to solid dissolved clarification, is heated up after filtering, after crystallization, filters to obtain solid E；6）Solid E is added in ethanol water, hydrochloric acid is added, is refined, crystallization and filtration, gained solid is Doxycycline Hyclate.The present invention is not only environmentally friendly, and the Doxycycline Hyclate rate of recovery is up to 92 95%.
Description
Technical field
The present invention relates to pharmaceutical technology field, in particular it relates to which a kind of reclaim salt from Doxycycline Hyclate refinement mother liquor
The method of sour Doxycycline.
Background technology
Doxycycline Hyclate is a kind of semi-synthetic tetracycline antibiotics of wide spectrum, to gram-positive bacteria, Gram-negative
Bacterium and Chlamydia are effective, are clinically used for respiratory tract infection, infection of biliary tract.Tonsillitis, lymphnoditis, cellulitis, old age are slow
The treatment of property bronchitis, Eaton agent pneumonia, syphilis, gonorrhoea, typhus, cholera, relapsing fever, pernicious malaria and hook end spiral
The prevention of body, the prophylactic as traveler's diarrhea can be also taken in short term.The aqueous solubility is strong, good absorbing, and distribution is wide, clinical
It is good using more and effect.
At present, the preparation of Doxycycline Hyclate is former by starting of 11 alpha-chloro -6- methine terramycin tosilate
Material, hydrogenated reduction, α -6- doxycycline sulfosalicylates are generated into salt, then α -6- doxycyclines are generated through alkalization
Alkali, finally refined in ethanol with hydrochloric acid, generate Doxycycline Hyclate, the liquid refined after filtering off product is refinement mother liquor.
Doxycycline Hyclate refinement mother liquor solvent is ethanol, contains 2-3% Doxycycline Hyclates in refinement mother liquor, 2% or so
6 β Doxycyclines and other a small amount of impurity, 6 more β Doxycyclines can be contained in regenerant obtained by direct concentration and recovery.No
Meet pharmacopoeial requirements, it is impossible to meet use demand.
The content of the invention
In order to improve, the Doxycycline Hyclate that is remained in Doxycycline Hyclate refinement mother liquor prepared by above-mentioned technology is high to be lacked
Fall into, the invention provides a kind of preparation method that Doxycycline Hyclate is reclaimed from Doxycycline Hyclate mother liquor of high-recovery, we
After method recovery, gained Doxycycline Hyclate contains a small amount of 6 β Doxycyclines, meets pharmacopoeial requirements.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention is：
The present inventor has found by research, by following processing step, can significantly reclaim in Doxycycline Hyclate mother liquor
Doxycycline Hyclate, and obtain the Doxycycline Hyclate of high-purity.
A kind of method that Doxycycline Hyclate is reclaimed in refinement mother liquor from Doxycycline Hyclate, comprises the following steps：
1）Sulfosalicylic acid is added into Doxycycline Hyclate refinement mother liquor to be handled, is stood still for crystals, and is carried out to separating out solid A
Filtering；
2）Ethanol water is added to solid A is filtered out, mashing washing is carried out, filters out solid B；
3）Solid B is added in ethanol water, ammoniacal liquor is added dropwise to solid dissolved clarification, is heated up after filtering, after crystallization, filters to obtain solid
C；
4）Solid C is added in ethanol water, hydrochloric acid, which is added dropwise, makes its dissolving, adds sulfosalicylic acid, solid to separating out after crystallization
Body D is filtered；
5）Solid D is added in ethanol water, ammoniacal liquor is added dropwise to solid dissolved clarification, is heated up after filtering, after crystallization, filters to obtain solid
E；
6）Solid E is added in ethanol water, hydrochloric acid is added, is refined, crystallization and filtration, gained solid is that how western hydrochloric acid is
Ring element.
Step 1）In, the sulfosalicylic acid addition is that every cubic metre of refinement mother liquor need to add 50-100kg sulfosalisylics
Acid, 20-60 DEG C of reaction temperature, stir 20-60min.
Step 2）In, the concentration of volume percent of the ethanol water is 40-60%, and it is solid masses kg to add volume L
3-5 times, mashing wash time is 20-40min.
Step 3）In, the concentration of volume percent of ethanol water is 55-70%, adds the 2- that volume L is solid masses kg
4 times, ammonia concn 9-15%, it is added dropwise during ammoniacal liquor and controls 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated into 30-50
DEG C, 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, is filtered.
Step 4）In, the concentration of volume percent of the ethanol water is 55-70%, and it is solid masses kg to add volume L
2-4 times, with salt acid for adjusting pH 1-3, sulfosalicylic acid addition is 0.9 times of solid masses, 20-60 DEG C of controlling reaction temperature.
Step 5）In, the concentration of volume percent of the ethanol water is 55-70%, and it is solid masses kg to add volume L
2-4 times, ammonia concn 9%-15%, be added dropwise during ammoniacal liquor and control 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated to
30-50 DEG C, about 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, is filtered.
Step 6）In, concentration of volume percent >=90% of the ethanol water, it is solid masses kg's to add volume L
3-5 times, hydrochloric acid adds 0.2 times that volume L is solid masses kg, and solid, which is dissolved in after ethanol, to be heated with stirring to 30~35 DEG C and add
Hydrochloric acid, separate out and be incubated 40~50 minutes at 60~65 DEG C after crystallizing, stirred crystallization 1-1.5 hours, cooling, extremely go out less than 25 DEG C
Material.
The described method that Doxycycline Hyclate is reclaimed from Doxycycline Hyclate refinement mother liquor, is comprised the following steps that：
1）Sulfosalicylic acid is added into Doxycycline Hyclate refinement mother liquor, sulfosalicylic acid addition is every cubic metre of refined mother
Liquid need to add 50-100kg sulfosalicylic acids, 20-60 DEG C of reaction temperature, stir 20-60min, be cooled to room temperature, stand still for crystals,
Filtered to separating out solid A；
2）To the 40-60% ethanol solutions for filtering out solid A 3-5 times of solid masses of addition, mashing washing 20-40min is carried out, is filtered out
Solid B；
3）Solid B is dissolved in the 55-70% ethanol of 2-4 times of volume, is sufficiently stirred into grout shape, be cooled to 0~5 DEG C, ammonia is added dropwise
Water, ammonia concn 9%-15%, it is added dropwise during ammoniacal liquor and controls 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated into 30-50
DEG C, about 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, filters to obtain solid C；
4）Solid C is dissolved in the 55-70% ethanol of 2-4 times of volume, adds sulfosalicylic acid, pH1-3, sulfo group are adjusted with hydrochloric acid
Salicylic acid addition is 0.9 times of solid masses, 20-60 DEG C of reaction temperature, stirs 15-30min, is cooled to room temperature, stands still for crystals,
Filtered to separating out solid D；
5）Solid D is dissolved in the 55-70% ethanol of 2-4 times of volume, is sufficiently stirred 2-3 hours, while be cooled to 0-5 DEG C, be added dropwise
Ammoniacal liquor, ammonia concn 9%-15%, it is added dropwise during ammoniacal liquor and controls 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated into 30-
50 DEG C, 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, filters to obtain solid E；
6）The concentration that solid E is dissolved in 3-5 times of volume is higher than in 90% ethanol, is heated with stirring to 30~35 DEG C, adds 0.2 times of body
Long-pending hydrochloric acid, 40~50min, stirred crystallization 1-1.5h are incubated at 60~65 DEG C after separating out crystallization, cooling, is extremely gone out less than 25 DEG C
Material, gained solid is Doxycycline Hyclate.
Beneficial effect：Compared with prior art, it is how western that hydrochloric acid is reclaimed in the refinement mother liquor of the invention from Doxycycline Hyclate
The method of ring element, Doxycycline Hyclate refinement mother liquor are recycled well, are compared to the ring directly caused by discharge
Border is polluted, and application of the invention is not only environmentally friendly, and the Doxycycline Hyclate rate of recovery reaches 92-94%.The hydrochloric acid that the present invention reclaims is more
Western ring element purity is high, has reached the index of pharmacopeia.
Brief description of the drawings
Fig. 1 is Doxycycline Hyclate liquid phase testing result figure prepared by embodiment 1；
Fig. 2 is Doxycycline Hyclate liquid phase testing result figure prepared by embodiment 2；
Fig. 3 is Doxycycline Hyclate liquid phase testing result figure prepared by embodiment 3.
Embodiment
It is further explained and described present invention by the following examples.But the embodiment provided is not understood that
To be construed as limiting to the scope of the present invention.
Embodiment 1
A kind of method that Doxycycline Hyclate is reclaimed in refinement mother liquor from Doxycycline Hyclate, step are as follows：
1）10L Doxycycline Hyclate refinement mother liquors are taken, add sulfosalicylic acid 750kg, reaction temperature is 48 DEG C, stirs 45min,
Room temperature is cooled to, is stood still for crystals, is filtered to separating out solid A.
2）To filter out solid A add 3 times of solid masses 40%（v:v）Ethanol solution, mashing washing 35min is carried out, is filtered out
Solid B.
3）Solid B is dissolved in the 60% of 3 times of volumes（v:v）In ethanol, grout shape is sufficiently stirred into, is cooled to 3 DEG C, is added dropwise
10% ammoniacal liquor, 10 DEG C of temperature is controlled, is filtered after stirring, filtrate is heated to 48 DEG C, be incubated 48min, cooling, spontaneous nucleation, to temperature
When spending 23 DEG C, solid C is filtered to obtain.
4）Solid C is dissolved in the 60% of 3 times of volumes（v:v）In ethanol, sulfosalicylic acid is added, with salt acid for adjusting pH 2.2,
Sulfosalicylic acid addition is 0.9 times of solid masses, 55 DEG C of reaction temperature, stirs 20min, is cooled to room temperature, stands still for crystals, right
Solid D is separated out to be filtered.
5）Solid D is dissolved in the 60% of 3 times of volumes（v:v）In ethanol, it is sufficiently stirred 2 hours, while is cooled to 2 DEG C, is added dropwise
10% ammoniacal liquor, 10 DEG C of temperature is controlled, is filtered after stirring, filtrate is heated to 48 DEG C, be incubated 50min, cooling, to crystallization all analysis
Go out, during to 23 DEG C of temperature, filter to obtain solid E.
6）Solid E is dissolved in the 95% of 3 times of volumes（v:v）In ethanol, 32 DEG C are heated with stirring to, adds the salt of 0.2 times of volume
Acid, 40min is incubated at 63 DEG C after separating out crystallization, cooling, stirred crystallization 1h, to 22 DEG C of dischargings, gained solid is the how western ring of hydrochloric acid
Element, which is given money as a gift, weighs 0.258kg, the rate of recovery 92.4%.
Gained Doxycycline Hyclate liquid phase testing result is as shown in figure 1, recovery Doxycycline Hyclate retention time is
12.183min, relative peak area 97.15%, the index of various pharmacopeia is reached.
Embodiment 2
A kind of method that Doxycycline Hyclate is reclaimed in refinement mother liquor from Doxycycline Hyclate, step are as follows：
1）10L Doxycycline Hyclate refinement mother liquors are taken, add sulfosalicylic acid 560kg, reaction temperature is 59 DEG C, stirs 30min,
Room temperature is cooled to, is stood still for crystals, is filtered to separating out solid A.
2）To filter out solid A add 3 times of solid masses 50%（v:v）Ethanol solution, mashing washing 20min is carried out, is filtered out
Solid B.
3）Solid B is dissolved in the 60% of 4 times of volumes（v:v）In ethanol, grout shape is sufficiently stirred into, is cooled to 4 DEG C, is added dropwise
15% ammoniacal liquor, 5 DEG C of temperature is controlled, is filtered after stirring, filtrate is heated to 50 DEG C, be incubated 30min, cooling, spontaneous nucleation, to temperature
When spending 20 DEG C, solid C is filtered to obtain.
4）Solid C is dissolved in the 60% of 4 times of volumes（v:v）In ethanol, sulfosalicylic acid is added, pH3.0 is adjusted with hydrochloric acid,
Sulfosalicylic acid addition is 0.9 times of solid masses, 59 DEG C of reaction temperature, stirs 25min, is cooled to room temperature, stands still for crystals, right
Solid D is separated out to be filtered.
5）Solid D is dissolved in the 60% of 4 times of volumes（v:v）In ethanol, it is sufficiently stirred 2.5 hours, while is cooled to 3 DEG C, drips
Add 15% ammoniacal liquor, control 5 DEG C of temperature, filtered after stirring, filtrate is heated to 33 DEG C, be incubated 25min, cooling, to crystallization all analysis
Go out, during to 22 DEG C of temperature, filter to obtain solid E.
6）Solid E is dissolved in the 92% of 5 times of volumes（v:v）In ethanol, 35 DEG C are heated with stirring to, adds the salt of 0.2 times of volume
Acid, 50min is incubated at 60 DEG C after separating out crystallization, cooling, stirred crystallization 1.5h, to 15 DEG C of dischargings, gained solid is that how western hydrochloric acid is
Ring element, which is given money as a gift, weighs 0.264kg, the rate of recovery 94.7%.
Gained Doxycycline Hyclate liquid phase testing result is as shown in Fig. 2 recovery Doxycycline Hyclate retention time is
12.481min, relative peak area 97.46%, the index of various pharmacopeia is reached.
Embodiment 3
A kind of method that Doxycycline Hyclate is reclaimed in refinement mother liquor from Doxycycline Hyclate, step are as follows：
1）10L Doxycycline Hyclate refinement mother liquors are taken, add sulfosalicylic acid 980kg, reaction temperature is 30 DEG C, stirs 60min,
Room temperature is cooled to, is stood still for crystals, is filtered to separating out solid A.
2）To filter out solid A add 4 times of solid masses 55%（v:v）Ethanol solution, mashing washing 40min is carried out, is filtered out
Solid B.
3）Solid B is dissolved in the 55% of 4 times of volumes（v:v）In ethanol, grout shape is sufficiently stirred into, is cooled to 3 DEG C, is added dropwise
13% ammoniacal liquor, 10 DEG C of temperature is controlled, is filtered after stirring, filtrate is heated to 45 DEG C, be incubated 30min, cooling, spontaneous nucleation, to temperature
When spending 18 DEG C, solid C is filtered to obtain.
4）Solid C is dissolved in the 55% of 4 times（v:v）In ethanol, sulfosalicylic acid is added, with salt acid for adjusting pH 1.1, sulfo group
Salicylic acid addition is 0.9 times of solid masses, 43 DEG C of reaction temperature, stirs 23min, is cooled to room temperature, stands still for crystals, to separating out
Solid D is filtered.
5）Solid D is dissolved in the 55% of 4 times（v:v）In ethanol, it is sufficiently stirred 2 hours, while is cooled to 4 DEG C, is added dropwise 13%
Ammoniacal liquor, 10 DEG C of temperature is controlled, is filtered after stirring, filtrate is heated to 47 DEG C, be incubated 36min, cooling, all separated out to crystallizing,
During to 15 DEG C of temperature, solid E is filtered to obtain.
6）Solid E is dissolved in the 93% of 3 times of volumes（v:v）In ethanol, 32 DEG C are heated with stirring to, adds the salt of 0.2 times of volume
Acid, 45min is incubated at 63 DEG C after separating out crystallization, cooling, stirred crystallization 1h, to 17 DEG C of dischargings, gained solid is the how western ring of hydrochloric acid
Element, which is given money as a gift, weighs 0.261kg, the rate of recovery 93.8%.
Gained Doxycycline Hyclate liquid phase testing result is as shown in figure 3, recovery Doxycycline Hyclate retention time is
12.372min, relative peak area 97.11%, the index of various pharmacopeia is reached.
Claims (8)
1. the method for Doxycycline Hyclate is reclaimed in a kind of refinement mother liquor from Doxycycline Hyclate, it is characterised in that including following
Step：
1）Sulfosalicylic acid is added into Doxycycline Hyclate refinement mother liquor to be handled, is stood still for crystals, and is carried out to separating out solid A
Filtering；
2）Ethanol water is added to solid A is filtered out, mashing washing is carried out, filters out solid B；
3）Solid B is added in ethanol water, ammoniacal liquor is added dropwise to solid dissolved clarification, is heated up after filtering, after crystallization, filters to obtain solid
C；
4）Solid C is added in ethanol water, hydrochloric acid, which is added dropwise, makes its dissolving, adds sulfosalicylic acid, solid to separating out after crystallization
Body D is filtered；
5）Solid D is added in ethanol water, ammoniacal liquor is added dropwise to solid dissolved clarification, is heated up after filtering, after crystallization, filters to obtain solid
E；
6）Solid E is added in ethanol water, hydrochloric acid is added, is refined, crystallization and filtration, gained solid is that how western hydrochloric acid is
Ring element.
2. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, step 1）In, the sulfosalicylic acid addition is that every cubic metre of refinement mother liquor need to add 50-100kg sulfosalisylics
Acid, 20-60 DEG C of reaction temperature, stir 20-60min.
3. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, step 2）In, the concentration of volume percent of the ethanol water is 40-60%, and it is solid masses kg to add volume L
3-5 times, mashing wash time is 20-40min.
4. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, step 3）In, the concentration of volume percent of ethanol water is 55-70%, adds the 2-4 that volume L is solid masses kg
Times, ammonia concn 9-15%, it is added dropwise during ammoniacal liquor and controls 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated into 30-50
DEG C, 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, is filtered.
5. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, step 4）In, the concentration of volume percent of the ethanol water is 55-70%, and it is solid masses kg to add volume L
2-4 times, with salt acid for adjusting pH 1-3, sulfosalicylic acid addition is 0.9 times of solid masses, 20-60 DEG C of controlling reaction temperature.
6. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, step 5）In, the concentration of volume percent of the ethanol water is 55-70%, and it is solid masses kg to add volume L
2-4 times, ammonia concn 9%-15%, be added dropwise during ammoniacal liquor and control 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated to
30-50 DEG C, about 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, is filtered.
7. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, step 6）In, concentration of volume percent >=90% of the ethanol water, add the 3- that volume L is solid masses kg
5 times, hydrochloric acid adds 0.2 times that volume L is solid masses kg, and solid, which is dissolved in after ethanol, to be heated with stirring to 30~35 DEG C and add salt
Acid, separate out and be incubated 40~50 minutes at 60~65 DEG C after crystallizing, stirred crystallization 1-1.5 hours, cooling, discharged to less than 25 DEG C.
8. reclaiming the method for Doxycycline Hyclate in the refinement mother liquor according to claim 1 from Doxycycline Hyclate, it is special
Sign is, comprises the following steps that：
1）Sulfosalicylic acid is added into Doxycycline Hyclate refinement mother liquor, sulfosalicylic acid addition is every cubic metre of refined mother
Liquid need to add 50-100kg sulfosalicylic acids, 20-60 DEG C of reaction temperature, stir 20-60min, be cooled to room temperature, stand still for crystals,
Filtered to separating out solid A；
2）To the 40-60% ethanol solutions for filtering out solid A 3-5 times of solid masses of addition, mashing washing 20-40min is carried out, is filtered out
Solid B；
3）Solid B is dissolved in the 55-70% ethanol of 2-4 times of volume, is sufficiently stirred into grout shape, be cooled to 0~5 DEG C, ammonia is added dropwise
Water, ammonia concn 9%-15%, it is added dropwise during ammoniacal liquor and controls 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated into 30-50
DEG C, about 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, filters to obtain solid C；
4）Solid C is dissolved in the 55-70% ethanol of 2-4 times of volume, adds sulfosalicylic acid, pH1-3, sulfo group are adjusted with hydrochloric acid
Salicylic acid addition is 0.9 times of solid masses, 20-60 DEG C of reaction temperature, stirs 15-30min, is cooled to room temperature, stands still for crystals,
Filtered to separating out solid D；
5）Solid D is dissolved in the 55-70% ethanol of 2-4 times of volume, is sufficiently stirred 2-3 hours, while be cooled to 0-5 DEG C, be added dropwise
Ammoniacal liquor, ammonia concn 9%-15%, it is added dropwise during ammoniacal liquor and controls 0-15 DEG C of temperature, after agitation and filtration, filtrate is heated into 30-
50 DEG C, 30-60min is incubated, cooling, spontaneous nucleation, when being less than 25 DEG C to temperature, filters to obtain solid E；
6）The concentration that solid E is dissolved in 3-5 times of volume is higher than in 90% ethanol, is heated with stirring to 30~35 DEG C, adds 0.2 times of body
Long-pending hydrochloric acid, 40~50min, stirred crystallization 1-1.5h are incubated at 60~65 DEG C after separating out crystallization, cooling, is extremely gone out less than 25 DEG C
Material, gained solid is Doxycycline Hyclate.
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Cited By (6)
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| CN108191692A (en) * | 2017-12-25 | 2018-06-22 | 安徽永生堂药业有限责任公司 | A kind of process for separation and purification of tetracycline antibiotics |
| CN110872241A (en) * | 2018-09-04 | 2020-03-10 | 山西卓联锐科科技有限公司 | Method for recovering sulfosalicylic acid and p-toluenesulfonic acid in doxycycline hydrogenation wastewater |
| CN111548284A (en) * | 2020-04-16 | 2020-08-18 | 海南通用康力制药有限公司 | Method for refining doxycycline hydrochloride |
| CN112645834A (en) * | 2020-12-21 | 2021-04-13 | 昆山华苏生物科技有限公司 | Preparation process of recovered hydride |
| CN114276271A (en) * | 2021-11-22 | 2022-04-05 | 新乡医学院三全学院 | Method for preparing doxycycline hydrochloride solid powder with different granularities |
| CN114835603A (en) * | 2022-06-17 | 2022-08-02 | 盐城苏海制药有限公司 | Synthesis method for directly synthesizing doxycycline hydrochloride from hydride |
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| CN110872241A (en) * | 2018-09-04 | 2020-03-10 | 山西卓联锐科科技有限公司 | Method for recovering sulfosalicylic acid and p-toluenesulfonic acid in doxycycline hydrogenation wastewater |
| CN111548284A (en) * | 2020-04-16 | 2020-08-18 | 海南通用康力制药有限公司 | Method for refining doxycycline hydrochloride |
| CN112645834A (en) * | 2020-12-21 | 2021-04-13 | 昆山华苏生物科技有限公司 | Preparation process of recovered hydride |
| CN114276271A (en) * | 2021-11-22 | 2022-04-05 | 新乡医学院三全学院 | Method for preparing doxycycline hydrochloride solid powder with different granularities |
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Application publication date: 20171201 |