CN211158691U - Chromatographic device for separating and purifying taxane substances - Google Patents
Chromatographic device for separating and purifying taxane substances Download PDFInfo
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- CN211158691U CN211158691U CN201921759605.3U CN201921759605U CN211158691U CN 211158691 U CN211158691 U CN 211158691U CN 201921759605 U CN201921759605 U CN 201921759605U CN 211158691 U CN211158691 U CN 211158691U
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- 229940123237 Taxane Drugs 0.000 title claims description 10
- DKPFODGZWDEEBT-QFIAKTPHSA-N taxane Chemical class C([C@]1(C)CCC[C@@H](C)[C@H]1C1)C[C@H]2[C@H](C)CC[C@@H]1C2(C)C DKPFODGZWDEEBT-QFIAKTPHSA-N 0.000 title abstract description 10
- 239000000126 substance Substances 0.000 title description 3
- 238000000926 separation method Methods 0.000 claims abstract description 63
- 238000000746 purification Methods 0.000 claims abstract description 28
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 26
- 238000012856 packing Methods 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 238000012546 transfer Methods 0.000 claims abstract description 6
- 239000012452 mother liquor Substances 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000003480 eluent Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000010963 304 stainless steel Substances 0.000 claims description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 3
- 230000000007 visual effect Effects 0.000 claims description 3
- 241001149649 Taxus wallichiana var. chinensis Species 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 229930012538 Paclitaxel Natural products 0.000 description 5
- 238000010828 elution Methods 0.000 description 5
- 229960001592 paclitaxel Drugs 0.000 description 5
- 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 description 5
- YWLXLRUDGLRYDR-UHFFFAOYSA-N 10-deacetylbaccatin Chemical compound CC(=O)OC12COC1CC(O)C(C(C(O)C1=C(C)C(O)CC3(O)C1(C)C)=O)(C)C2C3OC(=O)C1=CC=CC=C1 YWLXLRUDGLRYDR-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000005526 G1 to G0 transition Effects 0.000 description 4
- 230000016507 interphase Effects 0.000 description 4
- 239000012043 crude product Substances 0.000 description 3
- OVMSOCFBDVBLFW-VHLOTGQHSA-N 5beta,20-epoxy-1,7beta,13alpha-trihydroxy-9-oxotax-11-ene-2alpha,4alpha,10beta-triyl 4,10-diacetate 2-benzoate Chemical compound O([C@@H]1[C@@]2(C[C@H](O)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)O)C(=O)C1=CC=CC=C1 OVMSOCFBDVBLFW-VHLOTGQHSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- TYLVGQKNNUHXIP-MHHARFCSSA-N 10-deacetyltaxol Chemical compound O([C@H]1[C@H]2[C@@](C([C@H](O)C3=C(C)[C@@H](OC(=O)[C@H](O)[C@@H](NC(=O)C=4C=CC=CC=4)C=4C=CC=CC=4)C[C@]1(O)C3(C)C)=O)(C)[C@@H](O)C[C@H]1OC[C@]12OC(=O)C)C(=O)C1=CC=CC=C1 TYLVGQKNNUHXIP-MHHARFCSSA-N 0.000 description 1
- 229930014667 baccatin III Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000001965 increasing effect Effects 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- OVARTBFNCCXQKS-UHFFFAOYSA-N propan-2-one;hydrate Chemical compound O.CC(C)=O OVARTBFNCCXQKS-UHFFFAOYSA-N 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
- Epoxy Compounds (AREA)
Abstract
The utility model relates to a chinese yew deep-processing technical field, concretely relates to a chromatography device for taxane class material separation and purification. This chromatography device is including the pre-column, its top of pre-column is equipped with pre-column upper cover, its bottom is equipped with pre-column lower cover, pre-column lower cover has the separation column through the pipe connection of lower part, pre-column upper cover top is equipped with blast pipe and feed liquor pipe, the blast pipe is connected with the vacuum pump, the feed liquor union coupling has the transfer pump, the transfer pump is connected with chromatography mother liquor inlet tube and eluant inlet tube respectively through three-way solenoid valve, the pre-column middle part is equipped with first packing layer, separation column middle part is equipped with the second packing layer, its bottom is equipped with the drain pipe, drain pipe department installs the velocity of flow control. The utility model discloses to prior art's not enough, provide a simple structure is reasonable is used for chromatographic device of taxane class material separation and purification, solved current chromatography column and can't realize secondary purification and separation efficiency low problem, and can improve the separation and purification effect.
Description
Technical Field
The utility model relates to a chinese yew deep-processing technical field, concretely relates to a chromatography device for taxane class material separation and purification.
Background
After the branches and leaves of the taxus chinensis are leached and extracted, the content of the taxol in the extract can reach 0.3-0.5 percent generally, and can only reach 0.8-1.0 percent after degreasing treatment. However, the production of paclitaxel fine products usually requires the input content of the crude product to reach more than 10%, which requires the subsequent treatment of the paclitaxel crude product in terms of process, and usually, column chromatography separation is adopted to increase the content of paclitaxel in the crude product. The chromatographic column is generally a common glass tube or an organic glass tube, and the stationary phase and the mobile phase need to be selected differently according to different separation objects. A method for separating components by repeated distribution according to different distribution coefficients of each component in a sample mixture in a stationary phase (filler) and a mobile phase (eluent). At present, the extraction paste is separated and purified, except for primary separation and purification by using a silica gel filler, resin is also required to be used for secondary purification, and the conventional chromatographic column cannot smoothly realize secondary purification, filling, cleaning or unloading of the filler. In addition, the existing chromatographic separation column has no pressure increasing and reducing effect, so that the separation speed is low, and the separation working efficiency is very low.
SUMMERY OF THE UTILITY MODEL
The utility model discloses to prior art's not enough, provide a simple structure is reasonable is used for chromatographic device of taxane class material separation and purification, solved current chromatography column and can't realize secondary purification and separation efficiency low problem, and can improve the separation and purification effect.
The technical scheme of the utility model is realized like this: the utility model provides a chromatographic device for separation and purification of taxanes, includes the pre-column, its top of pre-column is equipped with pre-column upper cover, and its bottom is equipped with pre-column lower cover, its characterized in that, pre-column lower cover has the separation column through the pipe connection of lower part, pre-column upper cover top is equipped with blast pipe and feed liquor pipe, the blast pipe is connected with the vacuum pump, the feed liquor union coupling has the transfer pump, the transfer pump is connected with chromatography mother liquor inlet tube and eluent inlet tube respectively through three solenoid valve, pre-column middle part is equipped with first packing layer, separation column its middle part is equipped with the second packing layer, and its bottom is equipped with the drain pipe, flow rate control valve is installed to drain pipe department.
The top of the separation column is provided with an upper separation column sealing cover, the bottom of the separation column is provided with a lower separation column sealing cover, and the liquid outlet pipe is arranged on the lower separation column sealing cover.
And a sand core and a fixing ring are arranged below the second packing layer, and the sand core is clamped on the fixing ring.
The pre-column and the separation column are both made of 304 stainless steel materials, and an arc-shaped porous filler baffle is arranged below the inner part of the pre-column.
200-300 mesh silica gel particles are filled in the first filler layer, and R203 or R204 macroporous resin is filled in the second filler layer.
The guide pipe is provided with a visual cup for observation.
The utility model provides an existing defect among the background art, have following beneficial effect:
the utility model provides a chromatography device for separation and purification of taxane class material simple structure is reasonable, has solved the unable secondary purification and the low problem of separation efficiency of realizing of current chromatographic column, and can improve the separation and purification effect. The utility model discloses a set up pre-column and detached column to the separation degree to the taxane class material has been improved to the polyphone chromatography, has realized the secondary purification, and the parallel flow is smoothly loaded and is cleared up, has improved separation and purification's efficiency. Before chromatography, the vacuum pump is started to evacuate, so that fixed interphase bubbles are reduced, the uniformity of the bubbles is ensured, and in the elution process, the vacuum pump is used for pressurizing, so that the eluent can smoothly pass through the stationary phase, and the separation efficiency is greatly improved. Through changing the psammitolite, can realize the filtration demand of same chromatographic column to the material of different particle sizes, increase the application range of chromatographic column. An arc-shaped porous filler baffle is arranged below the inner part of the pre-column, so that the pressure of the filler on the filler baffle can be uniformly distributed, and the filler is ensured to be clean without dead angles.
Drawings
Fig. 1 is a schematic structural view of the present invention;
in the figure: 1-pre-column, 2-separation column, 3-guide tube, 4-liquid inlet tube, 5-liquid outlet tube, 6-liquid conveying pump, 7-chromatography mother liquid inlet tube, 8-eluent inlet tube, 9-pre-column upper sealing cover, 10-pre-column lower sealing cover, 11-separation column upper sealing cover, 12-separation column lower sealing cover, 13-flow rate control valve, 14-exhaust tube, 15-vacuum pump, 16-first packing layer, 17-second packing layer, 18-sand core, 19-fixing ring, 20-three-way electromagnetic valve, 21-packing baffle and 22-visual cup.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
The embodiment of the chromatography device for separation and purification of the taxane substances shown in fig. 1 comprises a pre-column 1, wherein the top of the pre-column 1 is provided with a pre-column upper sealing cover 9, the bottom of the pre-column 1 is provided with a pre-column lower sealing cover 10, the pre-column lower sealing cover 10 is connected with a separation column 2 through a lower guide pipe 3, the top of the pre-column upper sealing cover 9 is provided with an exhaust pipe 14 and a liquid inlet pipe 4, the exhaust pipe 14 is connected with a vacuum pump 15, and the vacuum pump 15 is a positive and negative pressure dual-purpose vacuum pump. The liquid inlet pipe 4 is connected with a liquid conveying pump 6, the liquid conveying pump 6 is respectively connected with a chromatography mother liquid inlet pipe 7 and an eluent inlet pipe 8 through a three-way electromagnetic valve 20, a first packing layer 16 is arranged in the middle of the pre-column 1, a second packing layer 17 is arranged in the middle of the separation column 2, a liquid outlet pipe 5 is arranged at the bottom of the separation column, and a flow speed control valve 13 is arranged at the position of the liquid outlet pipe 5. The top of the separation column 2 is provided with a separation column upper sealing cover 11, the bottom of the separation column 2 is provided with a separation column lower sealing cover 12, and the liquid outlet pipe 5 is arranged on the separation column lower sealing cover 12. A sand core 18 and a fixing ring 19 are arranged below the second filler layer 17, and the sand core 18 is clamped on the fixing ring 19. The pre-column 1 and the separation column 2 are both made of 304 stainless steel materials, and an arc-shaped porous filler baffle plate 21 is arranged below the inner part of the pre-column 1. 200-300 mesh silica gel particles are filled in the first filler layer 16, and R203 or R204 macroporous resin is filled in the second filler layer 17. The conduit 3 is provided with a visual cup 22 for observation.
The utility model discloses a working process is: during operation, 200-300 mesh silica gel particles are uniformly filled into the first filler layer 16 in the pre-column 1, and the column wall is knocked by a rubber hammer until the silica gel is dense. The macroporous resin R203 or R204 is made into a uniform slurry by high-concentration acetone, and is filled into the second filler layer 17 in the separation column 2. And preparing a high-concentration acetone solution as eluent for separation and purification. Then, paclitaxel extract is pumped from a chromatography mother liquor inlet pipe 7 into the upper part of the inner part of the column 1 for chromatography by an infusion pump 6. Before chromatography, the vacuum pump 15 is started to perform exhaust treatment on the pre-column 1 and the separation column 2, and the internal air is evacuated, so that fixed interphase bubbles are reduced, and the uniformity of the fixed interphase bubbles is ensured. During elution, an eluent inlet pipe is connected through a three-way electromagnetic valve 20, and 20% acetone-water solution is pumped in for gradient elution. And the flow rate control valve 13 is adjusted to control the flow rate of the effluent liquid. When the chromatography is started, the eluate without color does not need to be concentrated and recovered, and can be directly used for preparing the solution. In the chromatography process, the flow rate of eluate in each section is uniform, and the flow rate of the eluate can be properly reduced in the section changing process. The elution sequence of the eluate was 10-DAB segment → baccatin III segment → 10-DAT segment → CEP segment → PAC segment. Wherein 10-DAB is the main material section, and strict control is required for ensuring the purification and refining of the working procedure. And (4) concentrating the eluate of the 10-DAB section, and recrystallizing the eluate to obtain a 10-DAB semi-finished product according to a semi-finished product recrystallization technology. The utility model discloses a set up pre-column 1 and knockout column 2 to the polyphone chromatography has improved the degree of separation to the taxane class material, has realized the secondary purification, and the parallel flow is smoothly loaded and is cleared up, has improved separation and purification's efficiency. Before chromatography, the vacuum pump 15 is started to evacuate, so that fixed interphase bubbles are reduced, the uniformity of the bubbles is ensured, and in the elution process, the vacuum pump 15 is used for pressurizing, so that the eluent can smoothly pass through the stationary phase, and the separation efficiency is greatly improved. By replacing the sand core 18, the filtering requirements of the same chromatographic column on materials with different particle sizes can be met, and the application range of the chromatographic column is enlarged. An arc-shaped porous filler baffle 21 is arranged below the inner part of the pre-column 1, so that the pressure of the filler on the filler baffle 21 can be uniformly distributed, and the filler is ensured to be clean without dead angles.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention, and any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The utility model provides a chromatographic device for separation and purification of taxanes, includes pre-column (1), its top of pre-column (1) is equipped with pre-column upper seal cover (9), and its bottom is equipped with pre-column lower seal cover (10), its characterized in that, pre-column lower seal cover (10) is connected with separation column (2) through pipe (3) of lower part, pre-column upper seal cover (9) top is equipped with blast pipe (14) and feed liquor pipe (4), blast pipe (14) are connected with vacuum pump (15), feed liquor pipe (4) are connected with transfer pump (6), transfer pump (6) are connected with chromatography mother liquor inlet tube (7) and eluent inlet tube (8) respectively through three way solenoid valve (20), pre-column (1) middle part is equipped with first packing layer (16), separation column (2) are equipped with second packing layer (17) in the middle part, and their bottom is equipped with drain pipe (5), and a flow rate control valve (13) is arranged at the liquid outlet pipe (5).
2. The chromatography device for separation and purification of taxanes according to claim 1, wherein: the top of the separation column (2) is provided with a separation column upper sealing cover (11), the bottom of the separation column (2) is provided with a separation column lower sealing cover (12), and the liquid outlet pipe (5) is arranged on the separation column lower sealing cover (12).
3. The chromatography device for separation and purification of taxanes according to claim 1 or 2, wherein: a sand core (18) and a fixing ring (19) are arranged below the second filler layer (17), and the sand core (18) is clamped on the fixing ring (19).
4. The chromatography device for separation and purification of taxanes according to claim 3, wherein: the pre-column (1) and the separation column (2) are both made of 304 stainless steel materials, and an arc-shaped porous filler baffle (21) is arranged below the inner part of the pre-column (1).
5. The chromatography device for separation and purification of taxanes according to claim 4, wherein: 200-300 mesh silica gel particles are filled in the first packing layer (16), and R203 or R204 macroporous resin is filled in the second packing layer (17).
6. The chromatography device for separation and purification of taxanes according to claim 5, wherein: a visual cup (22) for observation is arranged on the conduit (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921759605.3U CN211158691U (en) | 2019-10-19 | 2019-10-19 | Chromatographic device for separating and purifying taxane substances |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921759605.3U CN211158691U (en) | 2019-10-19 | 2019-10-19 | Chromatographic device for separating and purifying taxane substances |
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| Publication Number | Publication Date |
|---|---|
| CN211158691U true CN211158691U (en) | 2020-08-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921759605.3U Expired - Fee Related CN211158691U (en) | 2019-10-19 | 2019-10-19 | Chromatographic device for separating and purifying taxane substances |
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| CN (1) | CN211158691U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653093A (en) * | 2022-04-19 | 2022-06-24 | 河南农业大学 | Extraction and purification device of polysaccharide |
-
2019
- 2019-10-19 CN CN201921759605.3U patent/CN211158691U/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653093A (en) * | 2022-04-19 | 2022-06-24 | 河南农业大学 | Extraction and purification device of polysaccharide |
| CN114653093B (en) * | 2022-04-19 | 2023-02-28 | 河南农业大学 | A polysaccharide extraction and purification device |
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Granted publication date: 20200804 |