CN109738550A - Continuous purification experimental provision - Google Patents
Continuous purification experimental provision Download PDFInfo
- Publication number
- CN109738550A CN109738550A CN201910138582.2A CN201910138582A CN109738550A CN 109738550 A CN109738550 A CN 109738550A CN 201910138582 A CN201910138582 A CN 201910138582A CN 109738550 A CN109738550 A CN 109738550A
- Authority
- CN
- China
- Prior art keywords
- branch
- sample
- sample introduction
- chromatographic column
- control valve
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000746 purification Methods 0.000 title claims abstract description 21
- 238000011097 chromatography purification Methods 0.000 claims abstract description 35
- 239000000945 filler Substances 0.000 claims description 33
- 238000004088 simulation Methods 0.000 claims description 6
- 238000001228 spectrum Methods 0.000 claims description 3
- 238000007445 Chromatographic isolation Methods 0.000 claims 2
- 238000004587 chromatography analysis Methods 0.000 abstract description 24
- 239000007788 liquid Substances 0.000 abstract description 21
- 238000002360 preparation method Methods 0.000 abstract description 16
- 238000011160 research Methods 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 402
- 238000002474 experimental method Methods 0.000 description 23
- 238000000034 method Methods 0.000 description 20
- 229930188195 rebaudioside Natural products 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- XQZXYNRDCRIARQ-LURJTMIESA-N iopamidol Chemical compound C[C@H](O)C(=O)NC1=C(I)C(C(=O)NC(CO)CO)=C(I)C(C(=O)NC(CO)CO)=C1I XQZXYNRDCRIARQ-LURJTMIESA-N 0.000 description 12
- 229960004647 iopamidol Drugs 0.000 description 12
- 230000005526 G1 to G0 transition Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 238000010521 absorption reaction Methods 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 229960004756 ethanol Drugs 0.000 description 6
- 238000011049 filling Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 241000883990 Flabellum Species 0.000 description 5
- 239000002250 absorbent Substances 0.000 description 5
- 230000002745 absorbent Effects 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 101001078143 Homo sapiens Integrin alpha-IIb Proteins 0.000 description 4
- 102100025306 Integrin alpha-IIb Human genes 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 230000001681 protective effect Effects 0.000 description 4
- QSRAJVGDWKFOGU-WBXIDTKBSA-N rebaudioside c Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]1(CC[C@H]2[C@@]3(C)[C@@H]([C@](CCC3)(C)C(=O)O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)CC3)C(=C)C[C@]23C1 QSRAJVGDWKFOGU-WBXIDTKBSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010835 comparative analysis Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229930182478 glucoside Natural products 0.000 description 3
- 150000008131 glucosides Chemical class 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 230000005654 stationary process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 241000723353 Chrysanthemum Species 0.000 description 2
- 235000007516 Chrysanthemum Nutrition 0.000 description 2
- 239000001512 FEMA 4601 Substances 0.000 description 2
- 239000001776 FEMA 4720 Substances 0.000 description 2
- HELXLJCILKEWJH-SEAGSNCFSA-N Rebaudioside A Natural products O=C(O[C@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1)[C@@]1(C)[C@@H]2[C@](C)([C@H]3[C@@]4(CC(=C)[C@@](O[C@H]5[C@H](O[C@H]6[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O6)[C@@H](O[C@H]6[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O6)[C@H](O)[C@@H](CO)O5)(C4)CC3)CC2)CCC1 HELXLJCILKEWJH-SEAGSNCFSA-N 0.000 description 2
- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- 238000002583 angiography Methods 0.000 description 2
- 238000013375 chromatographic separation Methods 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- HELXLJCILKEWJH-UHFFFAOYSA-N entered according to Sigma 01432 Natural products C1CC2C3(C)CCCC(C)(C(=O)OC4C(C(O)C(O)C(CO)O4)O)C3CCC2(C2)CC(=C)C21OC(C1OC2C(C(O)C(O)C(CO)O2)O)OC(CO)C(O)C1OC1OC(CO)C(O)C(O)C1O HELXLJCILKEWJH-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 2
- 235000019796 monopotassium phosphate Nutrition 0.000 description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 2
- 230000009979 protective mechanism Effects 0.000 description 2
- HELXLJCILKEWJH-NCGAPWICSA-N rebaudioside A Chemical compound O([C@H]1[C@H](O)[C@@H](CO)O[C@H]([C@@H]1O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O HELXLJCILKEWJH-NCGAPWICSA-N 0.000 description 2
- 235000019203 rebaudioside A Nutrition 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 229940013618 stevioside Drugs 0.000 description 2
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 2
- 235000019202 steviosides Nutrition 0.000 description 2
- 229960004799 tryptophan Drugs 0.000 description 2
- GOJUJUVQIVIZAV-UHFFFAOYSA-N 2-amino-4,6-dichloropyrimidine-5-carbaldehyde Chemical group NC1=NC(Cl)=C(C=O)C(Cl)=N1 GOJUJUVQIVIZAV-UHFFFAOYSA-N 0.000 description 1
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 241000189115 Catananche Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 101000961414 Homo sapiens Membrane cofactor protein Proteins 0.000 description 1
- 102100039373 Membrane cofactor protein Human genes 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 244000228451 Stevia rebaudiana Species 0.000 description 1
- 235000006092 Stevia rebaudiana Nutrition 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PVBALTLWZVEAIO-UHFFFAOYSA-N diodone Chemical compound OC(=O)CN1C=C(I)C(=O)C(I)=C1 PVBALTLWZVEAIO-UHFFFAOYSA-N 0.000 description 1
- 229960001845 diodone Drugs 0.000 description 1
- 229930004069 diterpene Natural products 0.000 description 1
- -1 diterpene compound Chemical class 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- FEQSXXYJWMCXJX-FMYGVZKHSA-N fusicoccin j Chemical compound O([C@H]1[C@H](O)[C@H](C)[C@@H]\2CC[C@@H](C/2=C/[C@@]2(C)[C@@H](O)CC(=C21)C(C)C)COC)[C@H]1O[C@H](COC(C)(C)C=C)[C@@H](O)[C@H](O)[C@H]1O FEQSXXYJWMCXJX-FMYGVZKHSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 235000021096 natural sweeteners Nutrition 0.000 description 1
- 210000000944 nerve tissue Anatomy 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The present invention relates to chromatography purity field, especially a kind of continuous purification experimental provision.Including sample presentation pipeline, sample introduction pipeline, array chromatographic purification module and sample outlet pipe road, sample introduction pipeline includes sample introduction main road and sample introduction branch, the sample introduction end of chromatographic purification module is connect with sample introduction main road, the sample outlet end of chromatographic purification module is connect with sample outlet pipe road, sample outlet pipe road is equipped with control valve III, one end of sample presentation pipeline is connect with sample, sample presentation pipeline passes through control valve I respectively and connect with the sample introduction main road of chromatographic purification module, each chromatographic purification module is correspondingly arranged several sample introduction branches, one end of sample introduction branch is connected with the sample introduction main road of corresponding chromatographic purification module, the other end of sample introduction branch is connect with the sample introduction branch of other chromatographic purification modules and sample outlet pipe road, the junction on sample introduction branch and sample outlet pipe road is located at the entrance of control valve, control valve II is equipped in sample introduction branch.Research and analysis suitable for all current liquid chromatogram separating-purifying preparation processes.
Description
Technical field
The present invention relates to chromatography purity field, especially a kind of continuous purification experimental provision.
Background technique
Chromatographic purification technology has become one of most important separating and purifying technology at present, is developed to from early 20th century
The present theoretically develops to non-linear chromatography from linear chromatography, then develops to system from analysis test-type chromatography in practice
Standby type and mass production type.
Liquid phantom preparing chromatogram is not the simple amplification for analyzing chromatography, and the two has many differences.Liquid phase preparative scale chromatography
The factor mainly considered is purity, yield, production cycle, operating cost of target product etc..And the optimization of its preparation process
It is to guarantee that equipment can achieve the premise of desired effect.So before the production of preparative equipment to the simulation of its preparation process and
Research becomes the most important thing.
Preparation process mainly includes that the columnar structures of chromatographic column, filler, column filling mode method, mobile phase pass through chromatographic column
When pressure, flow etc..Analog chromatogram preparation process can make people more deeply, intuitively recognize and find in practical life
The process of chromatographic separation and purification and the problem of being likely to occur in production, and then optimize preparation process, reach and save the development time, selectes
Solvent and stationary phase, while it is durable to stablize preparation process more, reduces cost and accelerates its equipment color commercialization.
Early stage preparative scale chromatography equipment for purifying realizes scale, staff rule of thumb and simply tests mostly
Determine preparation process, obtained resultant error is larger, and consuming time is long, at high cost.Later period occur to preparation work
The analog study equipment of skill, be mostly preparative equipment manufacturer be research its meet oneself the with clearly defined objective experiment of apparatus and process and set
Standby, function is relatively single, and what can only be fixed studies the chromatographic separation and purification technique of certain or single classification substance, can not accomplish
Research to general preparation process.
Summary of the invention
It is an object of the invention to solve the above-mentioned problems in the prior art, a kind of continuous purification experiment dress is proposed
It sets, it is suitable for the research and analysis of all current liquid chromatogram separating-purifying preparation processes.
The technical scheme is that
A kind of continuous purification experimental provision, wherein including sample presentation pipeline, sample introduction pipeline, array chromatographic purification module
With sample outlet pipe road, sample introduction pipeline includes sample introduction main road and sample introduction branch, sample introduction end and the sample introduction main road of chromatographic purification module
Connection, the sample outlet end of chromatographic purification module are connect with sample outlet pipe road, and sample outlet pipe road is equipped with control valve III, sample presentation pipeline
One end is connect with sample, and sample presentation pipeline passes through control valve I respectively and connect with the sample introduction main road of chromatographic purification module, respectively
Chromatographic purification module is correspondingly arranged several sample introduction branches, one end of sample introduction branch and corresponding chromatographic purification module
The connection of sample introduction main road, the other end of sample introduction branch are connect with the sample introduction branch of other chromatographic purification modules and sample outlet pipe road,
The junction on sample introduction branch and sample outlet pipe road is located at the entrance of control valve, is equipped with control valve II in sample introduction branch.
The chromatographic purification module includes chromatographic column, is filled with filler in chromatographic column, chromatographic purification module is put
Set in insulating box, insulating box respectively with warm wind control feed system connect, temperature control system connect, temperature control system and
Warm wind controls feed system electrical connection.
The pipeline that the sample outlet end of the chromatographic purification module and corresponding sample introduction branch connect by control valve IV with
Comprehensive sample bottle connection.
Preferably, the present invention includes six groups of chromatographic purification modules, including chromatographic column A, chromatographic column B, chromatographic column C, color
Spectrum column D, chromatographic column E and chromatographic column F, chromatographic column A sample introduction branch include in be arranged in parallel branch AB, branch AC, branch AD,
The sample introduction branch of branch AE and branch AF, chromatographic column B include in be arranged in parallel branch BA, branch BC, branch BD, branch BE and
The sample introduction branch of branch BF, chromatographic column C include in the branch CA, branch CB, branch CD, branch CE and the branch CF that are arranged in parallel,
The sample introduction branch of chromatographic column D includes in branch DA, branch DB, branch DC, branch DE and the branch DF being arranged in parallel, chromatographic column E
Sample introduction branch include in the branch EA, branch EB, branch EC, branch ED and the branch EF that are arranged in parallel, the sample introduction branch of chromatographic column F
Road includes in branch FA, branch FB, branch FC, branch FD and the branch FE being arranged in parallel；
It is interconnected between the branch AB, branch CB, branch DB, branch EB and branch FB, the branch AC, branch
It is interconnected and connects between BC, branch DC, branch EC and branch FC, branch AD, branch BD, branch CD, branch ED and branch FD
Between be interconnected, between the branch AE, branch BE, branch CE, branch DE and branch FE be interconnected, branch AF, branch
Between BF, branch CF, branch DF and branch EF be interconnected, the branch BA, branch CA, branch DA, branch EA, branch FA it
Between be interconnected；
The sample outlet end of the chromatographic column A is connected to branch BA, branch CA, branch DA, branch EA, branch FA, chromatographic column B's
Sample outlet end is connected to branch AB branch CB, branch DB, branch EB, branch FB, the sample outlet end of chromatographic column C and branch AC, branch BC,
Branch DC, branch EC, branch FC connection, the sample outlet end and branch AD, branch BD, branch CD, branch ED, branch FD of chromatographic column D
Connection, the sample outlet end of chromatographic column E are connected to branch AE, branch BE, branch CE, branch DE, branch FE, the sample outlet end of chromatographic column F
It is connected to branch AF, branch BF, branch CF, branch DF, branch EF.
The pipe that the sample outlet end of pipeline, chromatographic column B that the sample outlet end of the chromatographic column A is connect with branch BA is connect with branch AB
Road, chromatographic column C sample outlet end connect with branch AC pipeline, chromatographic column D sample outlet end connect with branch AD pipeline, chromatographic column
The pipeline that the sample outlet end of pipeline, chromatographic column F that the sample outlet end of E is connect with branch AE is connect with branch AF passes through control valve IV respectively
It is connect with comprehensive sample bottle.
Beneficial effects of the present invention:
(1) multiple groups chromatographic purification module is set, and status is of equal value between each group of module, and can any control module
Working condition, it is not necessary to sequential control；
(2) sample and mobile phase can independent sample introduction, provide a variety of feasible schemes, while its sample for the research of preparation process
Product can switch between operational blocks which partition system, operator can arbitrarily be select and set according to requirement of experiment chromatographic column columnar structures,
Pressure, flow etc. when filler, column filling mode method, mobile phase pass through chromatographic column do not need complicated cumbersome operating procedure,
It saves many experiments time and obtains accurate experimental data；
(3) each chromatographic purification module can individually go out sample, and the sample that goes out of comprehensive sample, tool can also be carried out by branch
The sample loading mode that goes out of body can be determining according to the experimental method of experiment purpose and experimenter's setting；
(4) intelligence degree is high, and experimental result is accurate, at the same will not because of laboratory sample Type Change and replace experiment
Instrument reduces cost；
(5) setting and chromatographic apparatus interface, can be according to setting real-time monitoring refining effect.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention in embodiment 1.
In figure: 1 sample bottle A；2 by sample bottle B；3 sample presentations pump A；4 sample presentations pump B；5 sample bottle A；6 sample bottle B；7 samples
Product bottle C；8 sample bottle D；9 sample bottle E；10 sample bottle F；11 comprehensive sample bottles；12 warm winds control feed system；13 chromatographic column A；
14 chromatographic column B；5 chromatographic column C；16 chromatographic column D；17 chromatographic column E；18 chromatographic column F；19 sample introduction branch AB；20 sample introduction branch AC；21
Sample introduction branch AD；22 sample introduction branch AE；23 sample introduction branch AF；24 control valve, II AB；25 control valve, II AC；26 control valve, II AD；
27 control valve, II AE；28 control valve, II AF；29 sample introduction branch BF；30 sample introduction branch BE；31 sample introduction branch BD；32 sample introduction branches
BC；33 sample introduction branch BA；34 control valve, II BF；35 control valve, II BE；36 control valve, II BD；37 control valve, II BC；38 control valves
ⅡBA；39 sample introduction branch CF；40 sample introduction branch CE；41 sample introduction branch CD；42 sample introduction branch CB；43 sample introduction branch CA；44 controls
II CF of valve；45 control valve, II CE；46 control valve, II CD；47 control valve, II CB；48 control valve, II CA；49 sample introduction branch DF；50 into
Sample branch DE；51 sample introduction branch DC；52 sample introduction branch DB；53 sample introduction branch DA；54 control valve, II DF；55 control valve, II DE；56
II DC of control valve；57 control valve, II DB；58 control valve, II DA；59 sample introduction branch EF；60 sample introduction branch ED；61 sample introduction branch EC；
62 sample introduction branch EB；63 sample introduction branch EA；64 control valve, II EF；65 control valve, II ED；66 control valve, II EC；67 control valves II
EB；68 control valve, II EA；69 sample introduction branch FE；70 sample introduction branch FD；71 sample introduction branch FC；72 sample introduction branch FB；73 sample introduction branch
Road FA；74 control valve, II FE；75 control valve, II FD；76 control valve, II FC；77 control valve, II FB；78 control valve, II FA；79 controls
I AL of valve；80 control valve, I AY；81 control valve, I BL；82 control valve, I BY；83 control valve, I CL；84 control valve, I CY；85 control valves I
DL；86 control valve, I DY；87 control valve, I EL；88 control valve, I EY；89 control valve, I FL；90 control valve, I FY；91 control valve, III A；92
III B of control valve；93 control valve, III C；94 control valve, III D；95 control valve, III E；96 control valve, III F；97 control valve, IV F；98 controls
IV E of valve；99 control valve, IV D；100 control valve, IV C；101 control valve, IV B；102 control valve, IV A.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and examples.
Embodiment 1
As shown in Figure 1, continuous purification experimental provision described in the present embodiment includes two groups of samples and six groups of chromatographies
Purify module, wherein two groups of samples are contained in respectively in sample bottle A1 and in sample bottle B2, chromatography purity mould
Block respectively includes chromatographic column A13, chromatographic column B14, chromatographic column C15, chromatographic column D16, chromatographic column E17 and chromatographic column F18, chromatographic column
It is inside equipped with filler, the filling kind in chromatographic column is arbitrarily select and set by experimenter according to requirement of experiment.Experiment dress
Setting further includes sample presentation pipeline, sample introduction pipeline and sample outlet pipe road, corresponding since the experimental provision includes two groups of samples
Equipped with two sample presentation pipelines, one end of sample presentation pipeline is connected to in sample bottle A1 with sample bottle B2 respectively.Sample introduction pipeline
Including sample introduction main road and sample introduction branch, wherein sample introduction branch is connect with the sample introduction end of each chromatographic column.The one end on sample outlet pipe road is assorted
The sample outlet end connection of column is composed, the other end is connected with corresponding sample bottle.
Two sample presentation pipelines pass through control valve I respectively and connect with the sample introduction main road of each chromatographic column, are controlled whether by control valve I
Sample is provided to chromatographic column, and which sample is provided.Two sample presentation pipelines pass through I AY80 of I AL79 of control valve and control valve respectively
It is connect with the sample introduction main road of chromatographic column A, two sample presentation pipelines pass through I BL81's of control valve and I B82 of control valve and chromatographic column B respectively
The connection of sample introduction main road, the sample introduction main road that two sample presentation pipelines pass through I CL83 of control valve and I CY84 of control valve and chromatographic column C respectively connect
It connects, two sample presentation pipelines pass through I DL85 of control valve respectively and I DY86 of control valve is connect with the sample introduction main road of chromatographic column D, two sample presentation pipes
Road passes through I EL87 of control valve respectively and I EY88 of control valve is connect with the sample introduction main road of chromatographic column E, and two sample presentation pipelines pass through respectively
I FL89 of control valve and I FY90 of control valve are connect with the sample introduction main road of chromatographic column F.
The sample outlet pipe road of each chromatographic column is equipped with control valve III, and the on-off on sample outlet pipe road is controlled by control valve III.Color
The sample outlet pipe road for composing column A is equipped with III A91 of control valve, and the sample outlet pipe road of chromatographic column B is equipped with III B92 of control valve, chromatographic column C's
Sample outlet pipe road is equipped with III C93 of control valve, and the sample outlet pipe road of chromatographic column D is equipped with III D94 of control valve, the sample outlet pipe of chromatographic column E
Road is equipped with III E95 of control valve, and the sample outlet pipe road of chromatographic column F is equipped with III F96 of control valve.
Each chromatographic column is equipped with several sample introduction branches being arranged in parallel, one end of sample introduction branch and corresponding chromatographic column
The connection of sample introduction main road, the other end of sample introduction branch are connect with the sample introduction branch of other chromatographic columns and sample outlet pipe road, realize chromatography
The connection of column and other chromatographic column sample introductions end and/or sample outlet end, sample introduction branch road are equipped with control valve II, are controlled by control valve II
The on-off of sample introduction branch processed.In the present embodiment, the sample introduction branch of chromatographic column A13 include in be arranged in parallel sample introduction branch AB19,
Sample introduction branch AC20, sample introduction branch AD21, sample introduction branch AE22 and sample introduction branch AF23, sample introduction branch AB19 are equipped with control valve
II AB24, sample introduction branch AC20 are equipped with II AC25 of control valve, and sample introduction branch AD21 is equipped with II AD26 of control valve, sample introduction branch
AE22 is equipped with II AE27 of control valve, and sample introduction branch AF23 is equipped with II AF28 of control valve.
The sample introduction branch of chromatographic column B14 includes in sample introduction branch BA33, the sample introduction branch BC32, sample introduction branch being arranged in parallel
BD31, sample introduction branch BE30 and sample introduction branch BF29, sample introduction branch BA33 are equipped with II BA38 of control valve, on sample introduction branch BC32
It is equipped with II BD36 of control valve equipped with II BC37 of control valve, sample introduction branch BD31, sample introduction branch BE30 is equipped with control valve II
BE35, sample introduction branch BF29 are equipped with II BF34 of control valve.
The sample introduction branch of chromatographic column C15 includes in sample introduction branch CA43, the sample introduction branch CB42, sample introduction branch being arranged in parallel
CD41, sample introduction branch CE40 and sample introduction branch CF39, sample introduction branch CA43 are equipped with II CA48 of control valve, on sample introduction branch CB42
It is equipped with II CD46 of control valve equipped with II CB47 of control valve, sample introduction branch CD41, sample introduction branch CE40 is equipped with control valve II
CE45, sample introduction branch CF39 are equipped with II CF44 of control valve.
The sample introduction branch of chromatographic column D16 includes in sample introduction branch DA53, the sample introduction branch DB52, sample introduction branch being arranged in parallel
DC51, sample introduction branch DE50 and sample introduction branch DF49, sample introduction branch DA53 are equipped with II DA58 of control valve, on sample introduction branch DB52
It is equipped with II DC56 of control valve equipped with II DB57 of control valve, sample introduction branch DC51, sample introduction branch DE50 is equipped with control valve II
DE55, sample introduction branch DF49 are equipped with II DF54 of control valve.
The sample introduction branch of chromatographic column E17 includes in sample introduction branch EA63, the sample introduction branch EB62, sample introduction branch being arranged in parallel
EC61, sample introduction branch ED60 and sample introduction branch EF59, sample introduction branch EA63 are equipped with II EA68 of control valve, on sample introduction branch EB62
It is equipped with II EC66 of control valve equipped with II EB67 of control valve, sample introduction branch EC61, sample introduction branch ED60 is equipped with control valve II
ED65, sample introduction branch EF59 are equipped with II EF64 of control valve.
The sample introduction branch of chromatographic column F18 includes in sample introduction branch FA73, the sample introduction branch FB72, sample introduction branch being arranged in parallel
FC71, sample introduction branch FD70 and sample introduction branch FE69, sample introduction branch FA73 are equipped with II FA78 of control valve, on sample introduction branch FB72
It is equipped with II FC76 of control valve equipped with II FB77 of control valve, sample introduction branch FC71, sample introduction branch FD70 is equipped with control valve II
FD75, sample introduction branch FE69 are equipped with II FE74 of control valve.
Between sample introduction branch AB19, sample introduction branch CB42, sample introduction branch DB52, sample introduction branch EB62 and sample introduction branch FB72
Be interconnected, sample introduction branch AC20, sample introduction branch BC32, sample introduction branch DC51, sample introduction branch EC61 and sample introduction branch FC71 it
Between be interconnected connect, sample introduction branch AD21, sample introduction branch BD31, sample introduction branch CD41, sample introduction branch ED60 and sample introduction branch
It is interconnected between FD70, sample introduction branch AE22, sample introduction branch BE30, sample introduction branch CE40, sample introduction branch DE50 and sample introduction branch
It is interconnected between the FE69 of road, sample introduction branch AF23, sample introduction branch BF29, sample introduction branch CF39, sample introduction branch DF49 and sample introduction
Between branch EF59 be interconnected, the sample introduction branch BA33, sample introduction branch CA43, sample introduction branch DA53, sample introduction branch EA63,
It is interconnected between sample introduction branch FA73.
At the same time, the sample outlet end of chromatographic column A13 and sample introduction branch BA33, sample introduction branch CA43, sample introduction branch DA53, into
Sample branch EA63, sample introduction branch FA73 connection, the sample outlet end and sample introduction branch AB19, sample introduction branch CB42, sample introduction of chromatographic column B14
Branch DB52, sample introduction branch EB62, sample introduction branch FB72 connection, the sample outlet end and sample introduction branch AC20, sample introduction branch of chromatographic column C15
Road BC32, sample introduction branch DC51, sample introduction branch EC61, sample introduction branch FC71 connection, the sample outlet end and sample introduction branch of chromatographic column D16
AD21, sample introduction branch BD31, sample introduction branch CD41, sample introduction branch ED60, sample introduction branch FD70 connection, chromatographic column E17's goes out sample
End is connected to sample introduction branch AE22, sample introduction branch BE30, sample introduction branch CE40, sample introduction branch DE50, sample introduction branch FE60, chromatography
The sample outlet end and sample introduction branch AF23, sample introduction branch BF29, sample introduction branch CF39, sample introduction branch DF49, sample introduction branch of column F19
EF59 connection.
By above-mentioned setting, realizes each chromatographic column and be individually composed one group of sample introduction and sample outlet pipe reason system, while every group
Intercommunity, arbitrariness and equivalence, by the control to control valve, the work shape of any control module are realized between pipe-line system
State can either realize sequential flowing of the sample between each spectrum column, and out-of-order flowing, i.e. sample also may be implemented
Any flowing in whole device can be realized under the control action of control valve.
In addition, as shown, pipeline and comprehensive sample bottle 11 that the sample outlet end of chromatographic column A13 is connect with sample introduction branch BA33
Connection, the connecting line are equipped with IV A102 of control valve；Pipeline that the sample outlet end of chromatographic column B14 is connect with sample introduction branch AB19 with
Comprehensive sample bottle 11 connects, which is equipped with IV B101 of control valve；The sample outlet end of chromatographic column C15 is connect with branch AC20
Pipeline connect with comprehensive sample bottle 11, the connecting line is equipped with IV C100 of control valve；The sample outlet end and branch of chromatographic column D16
The pipeline of AD21 connection is connect with comprehensive sample bottle 11, which is equipped with IV D99 of control valve；Chromatographic column E17's goes out sample
The pipeline connecting with branch AE22 is held to connect with comprehensive sample bottle 11, which is equipped with IV A98 of control valve；Chromatographic column
The pipeline that the sample outlet end of F19 is connect with branch AF23 is connect with comprehensive sample bottle 11, which is equipped with control valve IV
F97.IV off-state of control valve, realize each chromatographic column independently goes out sample；IV on-state of control valve, realizes comprehensive sample
Go out sample.Specific quadrat method out can be determined according to the experimental method that experiment purpose and experimenter set.
The device further includes insulating box, warm wind control feed system 12 and temperature control system, and six groups in the present embodiment
Chromatography purity module is arranged in insulating box, and insulating box is connect with warm wind control feed system respectively, temperature control system connects
It connects, while temperature control system is also connect with warm wind control feed system.It includes cabinet, several automatic controls that warm wind, which controls feed system,
Warm heat-generating pipe, flabellum, connecting shaft, motor and pipe line is sent, several temp auto-controlled heat-generating pipes and flabellum are arranged in cabinet, cabinet
Interior is closed space, and motor is connect by connecting shaft with flabellum, and one end of pipe line is sent to be connected to cabinet, the other end and perseverance
Incubator connection.Temp auto-controlled heat-generating pipe generates heat when working, motor drives flabellum rotation, temperature automatically controlled by flabellum rotating member
The heat that heat-generating pipe generates is full of entire cabinet, and moves up the intracorporal stream of hot air of case, and hot-air is along sending pipe line defeated
It send to insulating box.
Temperature control system includes temperature sensor and controller, and temperature sensor is arranged in insulating box, temperature sensing
Device is electrically connected with the controller, and controller is connect with temp auto-controlled heat-generating pipe.The temperature for the insulating box that temperature sensor arrives real-time detection
Degree is sent to controller, by the heating temperature of controller control temp auto-controlled heat-generating pipe, to ensure that the temperature in insulating box is permanent
It is fixed.The controller used in this implementation can be single-chip microcontroller, or control circuit is the prior art, is not done herein superfluous
It states.
In the present invention, the quantity of chromatographic purification module is not limited to six groups in the present embodiment, can be according to reality
Situation selects five groups, four groups, minimum two groups, can also select more multiple groups；Sample is also not necessarily limited to two kinds in the present embodiment,
It can also select more kinds of.
In order to prevent influence of the external environment to sample and interfere purification purity, each chromatographic column is mounted in insulating box,
The real-time adjusting that temperature is carried out by temperature control system, maintains each chromatographic column to be in optimal operating temperature range.It is permanent simultaneously
Mountable placement and compatible a variety of chromatographic columns, are convenient for changing in incubator.
By the device may be implemented to all product out it is multiple, repeatedly purify, while it is any between each chromatographic column
Switching and regulation, improve the precision of results sample, while improving purification efficiency, save a large amount of activity time.
The device provides stable, efficient experimental facilities to a variety of feasible schemes research of preparation process.Test people
Member can arbitrarily set experiment parameter, any to select stationary phase type etc. kinds of experiments method, provide for the research of preparation process
A possibility that a large amount of.By simulating preparation process, the effect of intuitive and accurate reflection preparation process, and have wide range of applications,
The equal analog of purifies and separates technique of chemicals, drug, biological products, it is not necessary to replace experiment because of the type of replacement sample and set
It is standby, save equipment early-stage study cost.In the following examples, the arrangement achieves to chemicals, drug and biological products
The simulation and experiment of purifies and separates technique.
Embodiment 2
The present embodiment continuously isolates and purifies chromatography processes using unit simulation Novel L-tryptophan of the present invention.
Tryptophan also known as 2- amino -3- indyl propionic acid are a kind of aromatic series, heterocycle, nonpolar a-amino acid.It is a kind of
The necessary amino acid of important nutrition, humans and animals itself cannot be synthesized, can only be obtained by food.It is widely used at present
The industries such as medical treatment, food, feed addictive and Agricultural Environmental Monitoring.
Continuous purification to L-Trp is simulated by using the present apparatus, is deleted in different stationary phases and process conditions
Lower, more efficient, the more environmentally protective public good route of a set of cost is developed in choosing, replaces traditional purifying technique.
The present embodiment uses 6 groups of chromatographic purification modules, and 10mm*250mm-5.0 μm of chromatography is configured in each module
One, column, one group of sample introduction pipeline, one group of sample outlet pipe road, while configuring high pressure sample presentation and pumping 2, pipeline is several.
Because the present embodiment only discusses stationary phase and flow velocity, pressure, flow, the shadow that temperature purifies L-Trp continuous chromatography
It rings, so mobile phase is used uniformly 50mmoL/L potassium dihydrogen phosphate, 10% methanol solution.
In the present embodiment, the filler in chromatographic column A is Applexion XA2041-NH4, and the filler in chromatographic column B is
Filler in Applexion XA3114-S04, chromatographic column C is Applexion XA2043, and the filler in chromatographic column D is
Filler in Applexion XA2014-22, chromatographic column E is R&H XAD1600, and the filler in chromatographic column F is any of the above group
It closes.
Simulated experiment the following steps are included:
One, unified flow, flow velocity, column temperature, pressure, adjustment chromatographic column go out sample sequence.
1, unified setting flow velocity 1m/min, flow 500ml/min, 40 DEG C of column temperature, sample presentation pressure 20mpa, Detection wavelength
278nm。
By 50mmoL/L potassium dihydrogen phosphate, 10% methanol solution is sent into six groups of chromatographies and is mentioned by sampling pump A and sample presentation pump B respectively
Pure module, six groups carry out purification & isolation movement simultaneously, sample bottle A5, sample bottle B6, sample bottle C7, sample bottle D8, sample bottle E9,
Sample bottle F10 is respectively collected the sample after purification & isolation.
It is finished to 6 groups of sample collections, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
2. unified setting flow velocity 1m/min, flow 500ml/min, 40 DEG C of column temperature, sample presentation pressure 20mpa, Detection wavelength
278nm。
Chromatographic column A column bottom efflux is entered in chromatographic column B by feeding branch BA, and sample bottle B6 collects sample.Chromatographic column C
Column bottom efflux is entered in chromatographic column D by feeding branch DC, and sample bottle D8 collects sample.Chromatographic column E column bottom efflux passes through
Charging branch FE enters in chromatographic column F, and sample bottle F10 collects sample.
It is finished to 3 groups of sample collections, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
3. unified setting flow velocity 1m/min, flow 500ml/min, 40 DEG C of column temperature, sample presentation pressure 20mpa, Detection wavelength
278nm。
Chromatographic column A, B, C, D, E, F sequence goes out sample, i.e. chromatographic column A column bottom efflux enters chromatography by feeding branch BA
In column B, while chromatographic column A column bottom goes out liquid and enters in comprehensive sample bottle 11 through IV A102 of control valve；Chromatographic column B column bottom efflux
It is entered in chromatographic column C by feeding branch CB, while chromatographic column B column bottom goes out liquid and enters comprehensive sample through IV B101 of control valve
In bottle 11；Chromatographic column C column bottom efflux is entered in chromatographic column B by feeding branch DC, while chromatographic column C column bottom goes out liquid through controlling
IV C100 of valve processed is entered in comprehensive sample bottle 11；Chromatographic column D column bottom efflux enters chromatographic column E by feeding branch EC
In, while chromatographic column D column bottom goes out liquid and enters in comprehensive sample bottle 11 through IV D99 of control valve；Chromatographic column E column bottom efflux passes through
Charging branch FE is entered in chromatographic column F, while chromatographic column E column bottom goes out liquid and enters in comprehensive sample bottle 11 through IV E98 of control valve；
Chromatographic column F column bottom efflux flows directly into sample bottle F10, at the same chromatographic column F column bottom go out liquid entered through IV F97 of control valve it is comprehensive
It closes in sample bottle 11.
It is finished to 2 groups of sample collections, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
4. experimenter arbitrarily adjusts chromatographic column and goes out sample sequence, to obtain different in next experimental procedure
Sample, and Concentration Testing is carried out, and record.
Two, obtain the optimal case that chromatographic column goes out sample sequence according to above-mentioned experimental result, select chromatographic column filler, change
Flow, flow velocity, column temperature, pressure.
1. flow velocity 0.5m/min, flow 250ml/min are set, 30 DEG C of column temperature, sample presentation pressure 15mpa, Detection wavelength
278nm.Chromatographic column filler is constant.
It is finished to sample collection, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
2. flow velocity 1m/min, flow 500ml/min are set, 40 DEG C of column temperature, sample presentation pressure 20mpa, Detection wavelength 278nm.
Chromatographic column filler is constant.
It is finished to sample collection, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
3. flow velocity 1.5m/min, flow 750ml/min are set, 45 DEG C of column temperature, sample presentation pressure 25mpa, Detection wavelength
278nm.Chromatographic column filler is constant.
It is finished to sample collection, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
4. flow velocity 2m/min, flow 1000ml/min are set, 50 DEG C of column temperature, sample presentation pressure 25mpa, Detection wavelength 278nm.
Chromatographic column filler is non-discolouring.
It is finished to sample collection, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
5. unified setting flow velocity 2.5m/min, flow 1250ml/min, 55 DEG C of column temperature, sample presentation pressure 30mpa, Detection wavelength
278nm.Chromatographic column filler is constant.
It is finished to sample collection, it is unified that PH, conductivity and L-Trp Concentration Testing are carried out to sample, and record.
By to different chromatographic column filler selection modes, different in flow rate, flow, column temperature, sample presentation pressure and other parameters are directed to
Property experiment, obtain minimum cost, efficiency highest, most plus environmentally protective process program.
Embodiment 3
The present embodiment continuously isolates and purifies chromatography processes using unit simulation rebaudioside ingredient of the present invention.
Rebaudioside also known as stevioside, be catananche's STEVIA REBAUDIANA leaf in extract containing 10 kinds of ingredients
The mixture of diterpene glucoside belongs to tetracyclic diterpene compound according to the division of natural plants chemistry, and rebaudioside is a kind of natural
Sweetener, Gao Tiandu is low in calories, it is safe and non-toxic the features such as gradually receive the favor of people.10 kinds known to the rebaudioside
In glucoside, the content of various composition, mouthfeel and sugariness are different, wherein stevioside, content rebaudioside-A, and rebaudioside C's contains
Amount is higher, and accounts for 90% or more.The sugariness highest of content rebaudioside-A is approximately 450 times of sucrose.
Continuous purification to Lai Baodi C is simulated by using the present apparatus, deletes choosing in different stationary phases and process conditions,
Lower, more efficient, the more environmentally protective public good route of a set of cost is developed, traditional purifying technique is replaced.
The present embodiment uses 5 groups of chromatographic purification modules, and 16mm*500mm-5.0 μm of chromatography is configured in each module
One, column, one group of sample introduction pipeline, one group of sample outlet pipe road, while configuring high pressure sample presentation and pumping 2, pipeline is several.
Because the present embodiment only discusses under the conditions of different fixed phase stuffings and different flow, pressure, flow velocity, column temperature etc. to sweet tea
The influence that rebaudioside C ingredient continuous chromatography purifies in leaf chrysanthemum glucoside extracting solution.Mobile phase selection rebaudioside's extracting solution 200ml,
Dehydrated alcohol, deionized water.
In the present embodiment, the filler in chromatographic column A is macroporous absorbent resin ADS-8, and the filler in chromatographic column B is macropore suction
Filler in attached Resin A DS-7, chromatographic column C is macroporous absorbent resin ADS-17, and the filler in chromatographic column D is macroporous absorbent resin
Filler in AB-8, chromatographic column E is macroporous absorbent resin D-06.
Simulated experiment the following steps are included:
One, unified flow, flow velocity, column temperature, pressure, change chromatographic column filler and chromatographic column goes out sample sequence.
1. unified setting flow velocity 2BV/h, flow 50ml/min, 20 DEG C of column temperature, sample presentation pressure 10mpa.
By A, B, C, five chromatographic columns of D, E are filled full with above-mentioned filler, pump A using sample presentation with 10Mpa pressure for ethyl alcohol
It is pumped into chromatographic column and cleans stationary phase, until liquid out adds water no longer muddiness, then replace reagent, cleaned using deionized water
To no longer containing ethyl alcohol.Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and rebaudioside
When extracting solution is identical, stops absorption, record each chromatographic column adsorption saturation time.
2. unified setting flow velocity 2BV/h, flow 50ml/min, 20 DEG C of column temperature, sample presentation pressure 10mpa, will be in chromatographic column
Filler is arbitrarily adjusted to any combination of above-mentioned filler according to experimenter.
By A, B, C, the filler filling after five chromatographic column changes of D, E is full, using sample presentation pump A with 10Mpa pressure
Ethyl alcohol is pumped into chromatographic column and cleans stationary phase, until liquid out adds water no longer muddiness, reagent is then replaced, uses no ion
Water is cleaned to no longer containing ethyl alcohol.Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and sweet tea
When leaf chrysanthemum glucoside extracting solution is identical, stops absorption, record each chromatographic column adsorption saturation time.
3. unified setting flow velocity 2BV/h, flow 50ml/min, 20 DEG C of column temperature, sample presentation pressure 10mpa.It will be in chromatographic column
Filler is arbitrarily adjusted to any combination of above-mentioned filler according to experimenter.
By A, B, C, the filler filling after five chromatographic column changes of D, E is full, using sample presentation pump A with 10Mpa pressure
Ethyl alcohol is pumped into chromatographic column and cleans stationary phase, until liquid out adds water no longer muddiness, reagent is then replaced, uses no ion
Water is cleaned to no longer containing ethyl alcohol.
Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, and experimenter arbitrarily adjusts chromatographic column and goes out
Sample sequence.A, B, C may be selected, D, E sequence go out sample, and E, D, C also may be selected, and B, A sequence go out sample, A also may be selected, and D, E go out sample, side
Method is any.When efflux is identical as rebaudioside's extracting solution, stops absorption, record each chromatographic column adsorption saturation time.
Two, according to above-mentioned experiment, the optimal filling mode that chromatographic column goes out sample sequence optimal case and chromatographic column filler is obtained,
Change flow, flow velocity, column temperature, pressure.
1. flow velocity 1BV/h, flow 30ml/min are set, 10 DEG C of column temperature, sample presentation pressure 10mpa.
Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and rebaudioside's extracting solution
When identical, stop absorption, record each chromatographic column adsorption saturation time.
2. flow velocity 1.5BV/h, flow 35ml/min are set, 15 DEG C of column temperature, sample presentation pressure 12mpa.
Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and rebaudioside's extracting solution
When identical, stop absorption, record each chromatographic column adsorption saturation time.
3. flow velocity 2BV/h, flow 40ml/min are set, 20 DEG C of column temperature, sample presentation pressure 15mpa.
Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and rebaudioside's extracting solution
When identical, stop absorption, record each chromatographic column adsorption saturation time.
4. flow velocity 2.5BV/h, flow 45ml/min are set, 25 DEG C of column temperature, sample presentation pressure 20mpa.
Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and rebaudioside's extracting solution
When identical, stop absorption, record each chromatographic column adsorption saturation time.
5. flow velocity 3BV/h, flow 50ml/min are set, 30 DEG C of column temperature, sample presentation pressure 30mpa.
Rebaudioside's extracting solution is pumped into chromatographic column by sample presentation pump B to be adsorbed, to efflux and rebaudioside's extracting solution
When identical, stop absorption, record each chromatographic column adsorption saturation time.
Pass through to different chromatographic column filler selection modes and out sample sequence, different in flow rate, flow, column temperature, sample presentation pressure etc.
The specific aim of parameter is tested, and obtains minimum cost, efficiency highest, best environmentally protective process program.
Embodiment 4
Iopamidol is a kind of non-ionic water-soluble diodone, has good development effect, to vascular wall and nerve
Tissue toxicity is small, and adverse reaction is few, and property is stablized, applied widely, is mainly used for neuroradiology, angiography, CT inspection
Look into middle enhancing scanning, arthrography, digital subtraction angiography.
Iopamidol isolates and purifies difficulty, and reason is in crude product to contain the similar impurity of more structure.United States Pharmacopeia and Europe
Continent pharmacopeia has all done stringent restriction to its content.Currently, using macroporous absorbent resin absorption method, this method in Iopamidol production
Production cycle is long, and splitter effect is low, and the degree of automation is not high, and technology stability is bad, is unfavorable for the control of product quality.Simultaneously
A large amount of waste water can be also generated, environmental protection is unfavorable for.
Continuous purification to Iopamidol is simulated by using the present apparatus, deletes choosing in different stationary phases and process conditions,
Lower, more efficient, the more environmentally protective public good route of a set of cost is developed, traditional purifying technique is replaced.
This experiment uses 4 groups of chromatographic purification modules, and 250mm*4.6mm-5.0 μm of chromatography is configured in each module
One, column, one group of sample introduction pipeline, one group of sample outlet pipe road, while configuring high pressure sample presentation and pumping 2, pipeline is several.
In the present embodiment, mobile phase selects Iopamidol feed liquid (purity 230g/L), ultrapure water, industrial methanol.Stationary phase is
C18-1 (phosphorus content 13.7%), C18-2 (phosphorus content 11.5%), C18-3 (phosphorus content 9.3%), C18-4 (phosphorus content 8%).
C18-1 is loaded in chromatographic column A, C18-2 is loaded in B, and C18-3 is loaded in C, loads C18-3 in C in D.
Simulated experiment the following steps are included:
One, unified velocity, column temperature and sample presentation pressure change chromatographic column and go out sample sequence.
1. unified setting flow velocity 60ml/min, 20 DEG C of column temperature, sample presentation pressure 20mpa.
Mobile phase A is water, and B is methanol solution, Iopamidol feed liquid sampling volume 65ml.
Iopamidol feed liquid passes through chromatographic column A, chromatographic column B, chromatographic column C simultaneously, and chromatographic column D, duration 30min are collected respectively
Chromatographic column A, chromatographic column B, chromatographic column C, chromatographic column D sample outlet end sample, and detect comparative analysis.
2. unified setting flow velocity 60ml/min, 20 DEG C of column temperature, sample presentation pressure 20mpa.
Iopamidol feed liquid passes through chromatographic column A first, enters chromatographic column B through branch BA, then enter chromatography through branch CB
Column C, then chromatographic column D, duration 120min are entered through branch DC, chromatographic column D sample outlet end sample is collected, and detect comparative analysis.
3. unified setting flow velocity 60ml/min, 20 DEG C of column temperature, sample presentation pressure 20mpa.
Iopamidol feed liquid passes through chromatographic column D first, enters chromatographic column C through branch CD, then enter chromatography through branch BC
Column B enters chromatographic column A, duration 120min through branch AB again, collects chromatographic column A sample outlet end sample, and detect comparative analysis.
4. unified setting flow velocity 60ml/min, 20 DEG C of column temperature, sample presentation pressure 20mpa.
Iopamidol feed liquid is arbitrarily adjusted by chromatographic column sequence by experimenter.
5. unified setting flow velocity 60ml/min, 20 DEG C of column temperature, sample presentation pressure 20mpa.
Iopamidol feed liquid is arbitrarily adjusted by chromatographic column sequence by experimenter.
6. unified setting flow velocity 60ml/min, 20 DEG C of column temperature, sample presentation pressure 20mpa
Iopamidol feed liquid is arbitrarily adjusted by chromatographic column sequence by experimenter.
By flowing through the comparative experiments of different stationary phases to feed liquid, minimum cost, efficiency highest, most plus environmentally protective is obtained
Process program.
Claims (5)
1. a kind of simulation continuous purification experimental provision, it is characterised in that: including sample presentation pipeline, sample introduction pipeline, array chromatographic isolation
Purify module and sample outlet pipe road, sample introduction pipeline includes sample introduction main road and sample introduction branch, the sample introduction end of chromatographic purification module with
The connection of sample introduction main road, the sample outlet end of chromatographic purification module are connect with sample outlet pipe road, and sample outlet pipe road is equipped with control valve III, are sent
One end of sample pipeline is connect with sample, and sample presentation pipeline passes through the sample introduction master of control valve I Yu chromatographic purification module respectively
Road connection, each chromatographic purification module are correspondingly arranged several sample introduction branches, one end of sample introduction branch and corresponding chromatographic isolation
The sample introduction branch of the sample introduction main road connection of purification module, the other end of sample introduction branch and other chromatographic purification modules and out sample
The junction on piping connection, sample introduction branch and sample outlet pipe road is located at the entrance of control valve, is equipped with control valve in sample introduction branch
Ⅱ。
2. simulation continuous purification experimental provision according to claim 1, it is characterised in that: the chromatographic purification module
Including chromatographic column, filler is filled in chromatographic column, chromatographic purification module is placed in insulating box, insulating box respectively with warm wind
Feed system connection, temperature control system connection are controlled, temperature control system is electrically connected with warm wind control feed system.
3. continuous purification experimental provision according to claim 1, it is characterised in that: the chromatographic purification module goes out
Sample end is connect by control valve IV with comprehensive sample bottle with the pipeline that corresponding sample introduction branch connects.
4. continuous purification experimental provision according to claim 1, it is characterised in that: including six groups of chromatographic purification moulds
Block, including chromatographic column A, chromatographic column B, chromatographic column C, chromatographic column D, chromatographic column E and chromatographic column F, the sample introduction branch of chromatographic column A include
In branch AB, branch AC, branch AD, branch AE and the branch AF being arranged in parallel, the sample introduction branch of chromatographic column B includes setting in parallel connection
Branch BA, branch BC, branch BD, branch BE and the branch BF set, the sample introduction branch of chromatographic column C include in the branch being arranged in parallel
CA, branch CB, branch CD, branch CE and branch CF, the sample introduction branch of chromatographic column D include in branch DA, the branch being arranged in parallel
DB, branch DC, branch DE and branch DF, the sample introduction branch of chromatographic column E include in branch EA, the branch EB, branch being arranged in parallel
EC, branch ED and branch EF, the sample introduction branch of chromatographic column F include in branch FA, branch FB, the branch FC, branch being arranged in parallel
FD and branch FE；
It is interconnected between the branch AB, branch CB, branch DB, branch EB and branch FB, the branch AC, branch BC, branch
It is interconnected and connects between road DC, branch EC and branch FC, phase between branch AD, branch BD, branch CD, branch ED and branch FD
It is intercommunicated, it is interconnected between the branch AE, branch BE, branch CE, branch DE and branch FE, branch AF, branch BF, branch
Be interconnected between CF, branch DF and branch EF, the branch BA, branch CA, branch DA, branch EA, between branch FA mutually
Connection；
The sample outlet end of the chromatographic column A is connected to branch BA, branch CA, branch DA, branch EA, branch FA, and chromatographic column B's goes out sample
End is connected to branch AB branch CB, branch DB, branch EB, branch FB, the sample outlet end and branch AC, branch BC, branch of chromatographic column C
DC, branch EC, branch FC connection, the sample outlet end of chromatographic column D are connected to branch AD, branch BD, branch CD, branch ED, branch FD,
The sample outlet end of chromatographic column E is connected to branch AE, branch BE, branch CE, branch DE, branch FE, the sample outlet end and branch of chromatographic column F
AF, branch BF, branch CF, branch DF, branch EF connection.
5. continuous purification experimental provision according to claim 4, it is characterised in that: the sample outlet end and branch of the chromatographic column A
The pipeline of road BA connection, the pipeline that the sample outlet end of chromatographic column B is connect with branch AB, chromatographic column C sample outlet end connect with branch AC
Pipeline, chromatographic column D sample outlet end connect with branch AD pipeline, chromatographic column E the sample outlet end pipeline, the color that are connect with branch AE
The pipeline that the sample outlet end of spectrum column F is connect with branch AF passes through control valve IV respectively and connect with comprehensive sample bottle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910138582.2A CN109738550B (en) | 2019-02-25 | 2019-02-25 | Continuous purification experimental device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910138582.2A CN109738550B (en) | 2019-02-25 | 2019-02-25 | Continuous purification experimental device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109738550A true CN109738550A (en) | 2019-05-10 |
| CN109738550B CN109738550B (en) | 2024-04-16 |
Family
ID=66368335
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910138582.2A Active CN109738550B (en) | 2019-02-25 | 2019-02-25 | Continuous purification experimental device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109738550B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010038450A (en) * | 1999-10-25 | 2001-05-15 | 황우성 | Triple column recycling chromatography system and invention |
| US20020084222A1 (en) * | 2000-12-28 | 2002-07-04 | John Brann | Multi column chromatography system |
| CN101732890A (en) * | 2009-12-08 | 2010-06-16 | 辽宁科技大学 | Three-section simulated moving bed chromatography device |
| WO2013169537A1 (en) * | 2012-05-08 | 2013-11-14 | Dow Corning Corporation | Purification of chlorosilanes using chromatography |
| CN203989958U (en) * | 2014-07-15 | 2014-12-10 | 国家***第三海洋研究所 | Five district's series connection simulated movable bed chromatography devices |
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN106166402A (en) * | 2016-09-19 | 2016-11-30 | 辽宁科技大学 | A kind of moving bed imitation chromatogram separation facility |
| CN209606386U (en) * | 2019-02-25 | 2019-11-08 | 青岛众瑞智能仪器有限公司 | Continuous purification experimental provision |
-
2019
- 2019-02-25 CN CN201910138582.2A patent/CN109738550B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20010038450A (en) * | 1999-10-25 | 2001-05-15 | 황우성 | Triple column recycling chromatography system and invention |
| US20020084222A1 (en) * | 2000-12-28 | 2002-07-04 | John Brann | Multi column chromatography system |
| CN101732890A (en) * | 2009-12-08 | 2010-06-16 | 辽宁科技大学 | Three-section simulated moving bed chromatography device |
| WO2013169537A1 (en) * | 2012-05-08 | 2013-11-14 | Dow Corning Corporation | Purification of chlorosilanes using chromatography |
| CN203989958U (en) * | 2014-07-15 | 2014-12-10 | 国家***第三海洋研究所 | Five district's series connection simulated movable bed chromatography devices |
| CN104655768A (en) * | 2015-03-11 | 2015-05-27 | 天津博纳艾杰尔科技有限公司 | Automatic crude oil component separating device and application of automatic crude oil component separating device in separation wax and colloid in crude oil |
| CN106166402A (en) * | 2016-09-19 | 2016-11-30 | 辽宁科技大学 | A kind of moving bed imitation chromatogram separation facility |
| CN209606386U (en) * | 2019-02-25 | 2019-11-08 | 青岛众瑞智能仪器有限公司 | Continuous purification experimental provision |
Non-Patent Citations (2)
| Title |
|---|
| P. E. BARKER ET AL: "Chemical and Biochemical Separations Using Preparative and Large Scale Batch and Continuous Chromatography", CHEMICAL AND BIOCHEMICAL SEPARATIONS USING PREPARATIVE AND LARGE SCALE BATCH AND CONTINUOUS CHROMATOGRAPHY, vol. 17, no. 1, pages 1 - 65 * |
| 王晓飞 等: "多柱色谱技术进展", 色谱, vol. 37, no. 2, pages 123 - 131 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109738550B (en) | 2024-04-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US20180343812A1 (en) | Cannabis farming systems and methods | |
| CN103387489B (en) | Preparation method of high pure crocin and geniposide | |
| US6478966B2 (en) | System for extracting tetrodotoxin | |
| CN107216228B (en) | Eutectic solvent and method for extracting anthraquinone in rheum officinale | |
| CN101824018B (en) | Method for purifying dihydromyricetin | |
| CN105664527A (en) | Continuous chromatographic separation device and method using device | |
| CN209606386U (en) | Continuous purification experimental provision | |
| CN109738550A (en) | Continuous purification experimental provision | |
| CN101543686B (en) | Multifunctional microwave extraction apparatus for extracting fragrances and flavors from Chinese cigarette | |
| CN102382178B (en) | Separation method of sialoglycopeptide | |
| CN103869013A (en) | Online purification solid-phase extraction monolithic column and preparation method and purposes of monolithic column | |
| Liu et al. | Studies on chemical constituents from the flowers of Carthamus tinctorius L | |
| CN204789501U (en) | A multi -functional decontaminating column that is used for chain check spore toxin to detect | |
| CN111013189B (en) | Bacteriostatic substance separation and purification control system and method based on big data | |
| CN105017339B (en) | A kind of method that SMBC separation prepares raffinose and stachyose | |
| CN114516893B (en) | Fructus momordicae neoflavonoid compound, preparation method thereof and application thereof in bee attractant | |
| CN104788509A (en) | Process for extracting and preparing high-purity raffinose from degreased wheat germ | |
| CN110763771A (en) | Pretreatment method for measuring organochlorine pesticide and polychlorinated biphenyl in aquatic product culture water body | |
| CN104447950A (en) | Romidepsin separation and purification method | |
| CN104130127B (en) | A kind of process extracting chlorogenic acid from Herba Blumeae Balsamiferae | |
| CN114181778A (en) | Preparation method of ruminant trans-fatty acid | |
| Jiang et al. | Chemical constituents from root of Prismatomeris tetrandra | |
| CN106083919B (en) | Utilize the method for glycol-based silica gel extraction snakehead phosphatide | |
| CN220736609U (en) | Stevioside eluent separation recovery unit | |
| CN208065826U (en) | A kind of soybean lecithin extractor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information |
Address after: 266000 No. 1 Xueyue Road, Chengyang District, Qingdao City, Shandong Province Applicant after: Qingdao Zhongrui Intelligent Instrument Co.,Ltd. Address before: 266000 No. 1 Xueyue Road, Chengyang District, Qingdao City, Shandong Province Applicant before: QINGDAO ZHONGRUI INTELLIGENT INSTRUMENT Co.,Ltd. |
|
| CB02 | Change of applicant information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |