CN109384749A - A kind of purification process of taxol - Google Patents
A kind of purification process of taxol Download PDFInfo
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- CN109384749A CN109384749A CN201811603139.XA CN201811603139A CN109384749A CN 109384749 A CN109384749 A CN 109384749A CN 201811603139 A CN201811603139 A CN 201811603139A CN 109384749 A CN109384749 A CN 109384749A
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- taxol
- crude product
- methylene chloride
- purification process
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- 229930012538 Paclitaxel Natural products 0.000 title claims abstract description 102
- 229960001592 paclitaxel Drugs 0.000 title claims abstract description 102
- RCINICONZNJXQF-MZXODVADSA-N taxol Chemical compound O([C@@H]1[C@@]2(C[C@@H](C(C)=C(C2(C)C)[C@H](C([C@]2(C)[C@@H](O)C[C@H]3OC[C@]3([C@H]21)OC(C)=O)=O)OC(=O)C)OC(=O)[C@H](O)[C@@H](NC(=O)C=1C=CC=CC=1)C=1C=CC=CC=1)O)C(=O)C1=CC=CC=C1 RCINICONZNJXQF-MZXODVADSA-N 0.000 title claims abstract description 102
- 238000000746 purification Methods 0.000 title claims abstract description 32
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 144
- 239000012043 crude product Substances 0.000 claims abstract description 43
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003480 eluent Substances 0.000 claims abstract description 31
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004005 microsphere Substances 0.000 claims abstract description 12
- 239000000741 silica gel Substances 0.000 claims abstract description 12
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 12
- 238000010829 isocratic elution Methods 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 44
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 25
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 22
- 238000001953 recrystallisation Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 11
- 239000003208 petroleum Substances 0.000 claims description 11
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 235000016408 Podocarpus macrophyllus Nutrition 0.000 claims description 3
- 244000162450 Taxus cuspidata Species 0.000 claims description 3
- 235000009065 Taxus cuspidata Nutrition 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012530 fluid Substances 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- WCYAALZQFZMMOM-UHFFFAOYSA-N methanol;sulfuric acid Chemical compound OC.OS(O)(=O)=O WCYAALZQFZMMOM-UHFFFAOYSA-N 0.000 claims description 2
- 238000009991 scouring Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000945 filler Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000012065 filter cake Substances 0.000 abstract 1
- 238000004587 chromatography analysis Methods 0.000 description 8
- 238000004809 thin layer chromatography Methods 0.000 description 7
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D305/00—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
- C07D305/14—Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms condensed with carbocyclic rings or ring systems
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Epoxy Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of purification process of taxol, includes the following steps, 1) microsphere silica gel is taken, it is 1:2-4 by mass volume ratio, methylene chloride is added, homogenate is made, pours into chromatographic column and stands；2) the taxol crude product for taking content >=60% is 1:3-5 by mass volume ratio, is dissolved in methylene chloride, obtains crude product solution；3) methylene chloride, n-butanol and/or isopropanol are taken, is by volume 90-95:10-5 mixing, obtains eluent；4) crude product solution of step 2) is added in chromatographic column, carries out isocratic elution using the eluent of step 3), collects taxol section component；5) the taxol section component of step 4) is concentrated to dryness, recrystallizes, filters to take filter cake, be dried to obtain taxol finished product.Purification process of the present invention can easily and efficiently prepare high-purity taxol, and the filler used is at low cost, and production is of large quantities, be suitable for large-scale industrial production.
Description
Technical field
The present invention relates to field of medicine and chemical technology, in particular to a kind of purification process of taxol.
Background technique
Taxol is a kind of with the active natural organic-compound of broad spectrum anticancer.As new anticancer drug, how by
Step improves its production technology, and high-quality, low-cost taxol is prepared, is that those skilled in the art urgently solve for a long time
Certainly the problem of.
Chromatography is a kind of method highest to complex mixture separative efficiency that the mankind grasp up to now.With liquid phase
When chromatogram purification taxol, operation mostly carries out at room temperature, and filler used is inert media, the Nature comparison of mobile phase mostly
Mildly, be conducive to the natural activity for retaining taxol.
Currently, mainly using high performance liquid chromatography and crystallisation in large-scale production and preparation high-purity taxol technique
Two kinds of purification process are purified.Both purification process are complementary to one another, make the purification efficiency of taxol is higher, purification time compared with
It is short, and yield meets enterprise requirements.Wherein, high performance liquid chromatography is as purifying upstream process, to preparing high-purity taxol
There is irreplaceable role.However, the high performance liquid chromatography equipment investment being commonly used is expensive, instrument maintenance takes
With valuableness, purifying amount is smaller, seriously constrains the production capacity of high-purity taxol.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of purification process of taxol, can conveniently, fastly
Prompt prepares high-purity taxol, and the filler used is at low cost, and production is of large quantities, is suitable for large-scale industrial production.
The technical scheme is that a kind of purification process of taxol, includes the following steps,
1) microsphere silica gel is taken, is 1:2-4 by mass volume ratio, methylene chloride is added, homogenate is made, pours into quiet in chromatographic column
It sets；
2) taxol crude product is taken, is 1:3-5 by mass volume ratio, methylene chloride is added, dissolution obtains crude product solution；
3) methylene chloride, n-butanol and/or isopropanol are taken, is by volume 90-95:10-5 mixing, obtains eluent；
4) crude product solution of step 2) is added in chromatographic column, carries out isocratic elution using the eluent of step 3), collects
Taxol section component；
5) the taxol section component of step 4) is concentrated to dryness, is recrystallized, filtered, be dried to obtain taxol finished product.
Further, the partial size of the step 1) microsphere silica gel is 30-50 μm, and preferably 30 μm, the additional amount of homogenate is
Chromatographic column allows maximum loading amount, and the time of the standing is 12h.
Further, content >=60% of step 2) the taxol crude product.
Further, after step 4) isocratic elution, chromatographic column is cleaned, clear scouring water be methylene chloride, n-butanol and/
Or isopropanol, it is by volume 60-80:40-20 mixing, cleaning fluid volume is three times column volume, after cleaning, using one times
Column volume step 3) the eluent balance.
Further, the step 4) isocratic elution, under chromatographic solution contact plate 50-60, solvent is ethyl acetate: hexamethylene
=1:1-2 is developed the color using methanol sulphuric acid mixed liquor.
Further, the step 5) recrystallization is recrystallized using acetone, petroleum ether or n-hexane.
Specifically, the method for the step 5) recrystallization is, after taxol section component is concentrated to dryness, acetone is added, in 45-
55 DEG C dissolve, and petroleum ether or n-hexane are added under stirring condition, are cooled to room temperature, and growing the grain filters, dry, obtain recrystallization slightly
Product are repeated 3 times, then acetone is added into recrystallization crude product, dissolve in 45-55 DEG C, a volume times acetone is added under stirring condition
N-hexane, crystallization at room temperature filters, dry, obtains taxol finished product.
It has the advantages that by adopting the above technical scheme
1, purification process of the present invention utilizes single chromatographic system, using Conventional solvents according to unique solvent burden ratio, carries out
Gradient elution, can directly, quickly isolate high-purity taxol, until 99.5% or more, while there is higher product to receive
Rate, until 85% or more.If n-butanol and/or isopropanol ratios are higher than 10% in eluent, then it will appear larger polar impurity
With taxol together appearance, cause the separation of Japanese yew alkoxide component difficult, it is difficult to improve taxol purity；If n-butanol in eluent
And/or isopropanol ratios are lower than 5%, then effluent volume dramatically increases, while higher cost, is unfavorable for controlling taxol concentrate
Cost.
2, purification process of the present invention is easy to operate, and the waste material of generation is few, meanwhile, occupied area is small, and equipment investment is few, raw
Produce it is of large quantities, be suitable for large-scale industrial production.
3, the solvent that purification process of the present invention uses meets enterprise safety operation demand without risk is fired, in addition, use
Solvent is smaller to staff's injury, also helps staff's health.
4, purification process of the present invention uses volume ratio to wash for the methylene chloride of 90-95:10-5, n-butanol and/or isopropanol
De- liquid elutes small polar taxol, and big polar impurity is retained in chromatographic column, efficiently separates taxol and miscellaneous to reach
The purpose of matter.Methylene chloride, the n-butanol that the big polar impurity remained in chromatographic column is 60-80:40-20 using volume ratio
And/or isopropanol cleaning solution elutes, and to repeat loading, guarantees the purification effect of chromatographic column recycling, meets large quantities of
Measure the demand of purification of paclitaxel.
It is further described combined with specific embodiments below.
Specific embodiment
The equipment for not indicating concrete model in embodiment, usually equipment conventional in chemical field.
Embodiment 1
The purification process of the taxol of content 80%, includes the following steps,
A. 800g40 μm of microsphere silica gel, 1600ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: n-butanol=90:10 ratio prepares eluent 10L.
C. be taxol by mass volume ratio: the taxol crude product of 20g content 80% is dissolved in by methylene chloride=1:5
In 100ml methylene chloride.
D. the taxol crude product dissolved is added in chromatographic column and is parsed with eluent, utilize thin-layer chromatography chromatography
Method collects taxol section.After use, carried out clearly with the methylene chloride of 3 times of column volumes: n-butanol=80:20 solution 4.8L
It washes, then balances 1 times of column volume 1.6L with eluent.
E. the taxol section component of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 90ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 90ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
99.3%, the taxol 14.41g of purity 99.60%, taxol yield 89.43%.
Embodiment 2
The purification process of the taxol of content 70%, includes the following steps,
A. 800g30 μm of microsphere silica gel, 2400ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: n-butanol=93:7 ratio prepares eluent 15L.
C. be taxol by mass volume ratio: the taxol crude product of 20g content 70% is dissolved in 80ml by methylene chloride=1:4
In methylene chloride.
D. the taxol crude product dissolved is added in chromatographic column and is parsed with eluent, utilize thin-layer chromatography chromatography
Method collects taxol section.After use, carried out clearly with the methylene chloride of 3 times of column volumes: n-butanol=70:30 solution 4.8L
It washes, then balances 1 times of column volume 1.6L with eluent.
E. the taxol section component of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 80ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 80ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
101.0%, the taxol 12.35g of purity 99.62%, taxol yield 89.10%.
Embodiment 3
The purification process of the taxol of content 60%, includes the following steps,
A. 800g30 μm of microsphere silica gel, 3200ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: n-butanol=95:5 ratio prepares eluent 18L.
It c. is taxol: methylene chloride=1:3 ratio in mass volume ratio, by the taxol crude product of 20g content 60%
It is dissolved in 60ml methylene chloride, obtains crude product solution.
D. crude product solution is added in chromatographic column and is parsed with eluent, collect Japanese yew using thin-layer chromatography chromatography
Alcohol section component.After use, is cleaned with the methylene chloride of 3 times of column volumes: n-butanol=60:40 solution 4.8L, then used
Eluent balances 1 times of column volume 1.6L.
E. the taxol section component of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 90ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 90ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
99.7%, the taxol 10.31g of purity 99.53%, taxol yield 85.66%.
Embodiment 4
The purification process of the taxol of content 90%, includes the following steps,
A. 800g50 μm of microsphere silica gel, 2400ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: n-butanol=93:7 ratio prepares eluent 15L.
C. be taxol by mass volume ratio: the taxol crude product of 20g content 90% is dissolved in by methylene chloride=1:5
In 100ml methylene chloride.
D. the taxol crude product dissolved is added in chromatographic column and is parsed with eluent, utilize thin-layer chromatography chromatography
Method collects taxol section.After use, carried out clearly with the methylene chloride of 3 times of column volumes: n-butanol=75:25 solution 4.8L
It washes, then balances 1 times of column volume 1.6L with eluent.
E. the taxol section of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 90ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 90ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
101.2%, the taxol 16.70g of purity 99.76%, taxol yield 93.89%.
Embodiment 5
The purification process of the taxol of content 75%, includes the following steps,
A. 800g30 μm of microsphere silica gel, 3200ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: isopropanol=90:10 ratio prepares eluent 10L.
C. be taxol by mass volume ratio: the taxol crude product of 20g content 75% is dissolved in 60ml by methylene chloride=1:3
In methylene chloride.
D. the taxol crude product dissolved is added in chromatographic column and is parsed with eluent, utilize thin-layer chromatography chromatography
Method collects taxol section.After use, carried out clearly with the methylene chloride of 3 times of column volumes: isopropanol=60:40 solution 4.8L
It washes, then balances 1 times of column volume 1.6L with eluent.
E. the taxol section of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 90ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 90ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
99.5%, the taxol 13.35g of purity 99.6%, taxol yield 88.56%.
Embodiment 6
The purification process of the taxol of content 65%, includes the following steps,
A. 800g40 μm of microsphere silica gel, 2400ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: isopropanol=93:7 ratio prepares eluent 15L.
C. be taxol by mass volume ratio: the taxol crude product of 20g content 65% is dissolved in 80ml by methylene chloride=1:4
In methylene chloride.
D. the taxol crude product dissolved is added in chromatographic column and is parsed with eluent, utilize thin-layer chromatography chromatography
Method collects taxol section.After use, cleaned with the methylene chloride of 3 times of column volumes: isopropanol=65:35 solution
4.8L, then 1 times of column volume 1.6L is balanced with eluent.
E. the taxol section of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 90ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 90ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
89.8%, the taxol 11.57g of purity >=99.5%, taxol yield 87.93%.
Embodiment 7
The purification process of the taxol of content 60%, includes the following steps,
A. 800g50 μm of microsphere silica gel, 1600ml methylene chloride are taken, is poured into chromatographic column after homogenate is made, 12h is stood.
B. in methylene chloride: isopropanol=95:5 ratio prepares eluent 18L.
C. be taxol by mass volume ratio: the taxol crude product of 20g content 60% is dissolved in by methylene chloride=1:5
In 100ml methylene chloride.
D. the taxol crude product dissolved is added in chromatographic column and is parsed with eluent, utilize thin-layer chromatography chromatography
Method collects taxol section.After use, cleaned with the methylene chloride of 3 times of column volumes: isopropanol=80:20 solution
4.8L, then 1 times of column volume 1.6L is balanced with eluent.
E. the taxol section of collection is concentrated to dryness with Rotary Evaporators.
F. 90ml acetone is taken, 90ml petroleum is added under the taxol section component that 45-55 DEG C of dissolution is collected, stirring condition
Ether is cooled to room temperature, and growing the grain filters, dry, obtains recrystallization crude product, is repeated 3 times, then 90ml is added into recrystallization crude product
Acetone is dissolved in 45-55 DEG C, 90ml n-hexane is added under stirring condition, at room temperature crystallization, is filtered, dry, obtains content
99.4%, the taxol 10.28g of purity 99.62%, taxol yield 85.15%.
Claims (7)
1. a kind of purification process of taxol, which is characterized in that include the following steps,
1) microsphere silica gel is taken, is 1:2-4 by mass volume ratio, methylene chloride is added, homogenate is made, pours into chromatographic column and stands；
2) taxol crude product is taken, is 1:3-5 by mass volume ratio, methylene chloride is added, dissolution obtains crude product solution；
3) methylene chloride, n-butanol and/or isopropanol are taken, is by volume 90-95:10-5 mixing, obtains eluent；
4) crude product solution of step 2) is added in chromatographic column, carries out isocratic elution using the eluent of step 3), collects Japanese yew
Alcohol section component；
5) the taxol section component of step 4) is concentrated to dryness, is recrystallized, filtered, be dried to obtain taxol finished product.
2. purification process according to claim 1, which is characterized in that the partial size of the step 1) microsphere silica gel is 30-50 μ
M, preferably 30 μm, the additional amount of homogenate are that chromatographic column allows maximum loading amount, and the time of the standing is 12h.
3. purification process according to claim 1, which is characterized in that the content of step 2) the taxol crude product >=
60%.
4. purification process according to claim 1, which is characterized in that after step 4) isocratic elution, chromatographic column is cleaned,
Clear scouring water is methylene chloride, n-butanol and/or isopropanol, is by volume 60-80:40-20 mixing, cleaning fluid volume is three
Times column volume after cleaning, is balanced using one times of column volume step 3) eluent.
5. purification process according to claim 1, which is characterized in that the step 4) isocratic elution, chromatographic solution contact plate 50-
Under 60, solvent is ethyl acetate: hexamethylene=1:1-2, is developed the color using methanol sulphuric acid mixed liquor.
6. purification process according to claim 1, which is characterized in that the step 5) recrystallization uses acetone, petroleum ether
Or n-hexane is recrystallized.
7. purification process according to claim 6, which is characterized in that the method for the step 5) recrystallization is taxol
After Duan Zufen is concentrated to dryness, acetone is added, is dissolved in 45-55 DEG C, petroleum ether or n-hexane are added under stirring condition, is cooled to room
Temperature, growing the grain filter, dry, obtain recrystallization crude product, repeat 1-3 times, then acetone is added into recrystallization crude product, in 45-55 DEG C
It dissolves, the n-hexane of a volume times acetone is added under stirring condition, at room temperature crystallization, filter, it is dry, obtain taxol finished product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003143A (en) * | 2019-04-15 | 2019-07-12 | 云南汉德生物技术有限公司 | A method of extracting natural Japanese yew alcohol |
| CN110759877A (en) * | 2019-10-28 | 2020-02-07 | 海南紫杉园制药有限公司 | Process for preparing taxol |
| CN112645906A (en) * | 2020-12-29 | 2021-04-13 | 重庆臻源红豆杉发展有限公司 | Method for separating and purifying paclitaxel by high-efficiency chromatography |
| CN113717131A (en) * | 2021-08-27 | 2021-11-30 | 常熟纳微生物科技有限公司 | Separation and purification method of paclitaxel |
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