CN110018264A - The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation - Google Patents
The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation Download PDFInfo
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- CN110018264A CN110018264A CN201910393885.9A CN201910393885A CN110018264A CN 110018264 A CN110018264 A CN 110018264A CN 201910393885 A CN201910393885 A CN 201910393885A CN 110018264 A CN110018264 A CN 110018264A
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- 239000007788 liquid Substances 0.000 title claims abstract description 95
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007791 liquid phase Substances 0.000 title claims abstract description 22
- 238000005485 electric heating Methods 0.000 claims abstract description 44
- 238000000926 separation method Methods 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 12
- 239000012780 transparent material Substances 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000011144 upstream manufacturing Methods 0.000 claims description 6
- 230000033228 biological regulation Effects 0.000 claims description 3
- 230000005611 electricity Effects 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 24
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 238000002953 preparative HPLC Methods 0.000 abstract 1
- 239000003814 drug Substances 0.000 description 8
- 239000012264 purified product Substances 0.000 description 7
- AHWNMFUPCUBQQD-GXTPVXIHSA-N 1-[(2S,3S,4S,5R)-2,3,4-trifluoro-3,4-dihydroxy-5-(hydroxymethyl)oxolan-2-yl]pyrimidine-2,4-dione Chemical compound F[C@@]1([C@]([C@@](O[C@@H]1CO)(N1C(=O)NC(=O)C=C1)F)(O)F)O AHWNMFUPCUBQQD-GXTPVXIHSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000021715 photosynthesis, light harvesting Effects 0.000 description 2
- 230000002277 temperature effect Effects 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000004237 preparative chromatography Methods 0.000 description 1
- 238000004262 preparative liquid chromatography Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6034—Construction of the column joining multiple columns
- G01N30/6043—Construction of the column joining multiple columns in parallel
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a kind of multichannels to integrate liquid chromatogram column device, cabinet including front end opening, the coiling of cabinet rear wall is provided with electric heating tube, parallel interval is equipped with several analytic type performance liquid chromatographic columns in cabinet, that is analytical column, wall box is hinged with chamber door in open-mouth, and the top of each analytical column is respectively connected with out liquid and is in charge of；The bottom end of each analytical column passes through liquid separation mechanism connection feed liquor house steward respectively, and feed liquor house steward stretches out wall box and is connected with delivery pump；The invention also discloses the methods for the carry out liquid phase preparation for using the integrated liquid chromatogram column device of above-mentioned multichannel.The present invention combines analytical column good separating effect and prepares the big advantage of column sample volume, overcome that analytical column sample volume is small and preparative high performance liquid chromatography column prepares the poor defect of post separation effect, first separation is equivalent to former separating for several times, efficiently and conveniently, energy first separation goes out a variety of desired compounds, saves the separation costs of complex compound.
Description
Technical field
The present invention relates to high performance liquid preparative chromatography technical fields.
Background technique
The method of preparative liquid chromatography have become chemistry, biochemistry, medicine, industry, agricultural, environmental protection, commodity inspection and method inspection etc. learn
Important separate analytical technique in section field is essential in analytical chemistry, biochemistry and Environmental Chemistry worker's hand
Tool.By taking drug as an example, in Pharmacopoeia of People's Republic of China, share more than about 600 kinds of chemical synthetic drugs and more than about 400 kinds
The quality of Chinese medicine controls the method for applying liquid chromatogram, but quantity of sample handling and sample separation effect due to tradition preparation chromatography
Contradiction between rate is unresolved, preferably to be isolated and purified effect, must reduce quantity of sample handling, so that separation
It is cumbersome, increased costs, and then lead to the related drugs of some liquid phases preparation in the market the price is very expensive.
High performance liquid chromatograph is only equipped with analytical column (i.e. analytic type performance liquid chromatographic column), semi-preparative column or system at present
Standby column.Column is prepared when separating certain complex compounds, expected separating effect is often not achieved in separating effect.And analytical column energy
Reaching good separating effect, but since its sample volume is small, the time for needing to expend when being used to prepare is longer, and mobile phase is more,
So limiting its application in preparation liquid phase.To those skilled in the art, analytical column is used to carry out analysis test,
Column is prepared to be used to liquid phase preparation, analytical column and prepare column general be routine techniques understanding.
Summary of the invention
The purpose of the present invention is to provide a kind of multichannels to integrate liquid chromatogram column device, both has good separation effect
Fruit, and have the advantages that sample volume is big, preparative capacibility is high.
To achieve the above object, multichannel of the invention integrates the cabinet that liquid chromatogram column device includes front end opening, case
The coiling of body rear wall is provided with electric heating tube, and electric fan is equipped in the cabinet in front of electric heating tube, is put down in the cabinet in front of electric fan
Row interval is equipped with several analytical columns, and wall box is hinged with chamber door in open-mouth, and chamber door includes doorframe and pair in doorframe
Layer transparent material, has cavity between double transparent material；
The top of each analytical column is respectively connected with out liquid and is in charge of, and respectively liquid is in charge of and is collected for outlet tube beam out, outlet tube beam pass-out cabinet,
One in outlet tube beam goes out liquid and is in charge of for connecting external liquid chromatogram detector, and other liquid out in outlet tube beam are in charge of
It is passed through in the collection vessel outside cabinet；
The bottom end of each analytical column passes through liquid separation mechanism connection feed liquor house steward respectively, and feed liquor house steward stretches out wall box and and transport Stream
The delivery pump of dynamic phase is connected；
Electric heating tube and electric fan are connected with an electric control gear, and electric control gear is connected with display screen and temperature sensor, electricity
Control device and display screen are respectively positioned on cabinet exterior, and temperature sensor is located in the box body portion.
It is equipped with metal perforated plate in cabinet between the analytical column and electric fan, is evenly distributed on metal perforated plate multiple small
Hole, metal perforated plate is symmetrical above and below set there are two.
Analytical column spacing side by side is equipped with multiple, and any one of the liquid separation mechanism is using following two structure:
A, liquid separation mechanism includes multiple-way valve, and multiple-way valve has an inlet and a several liquid outlets, the liquid outlet of multiple-way valve with point
It analyses column and corresponds connection；The inlet of multiple-way valve is connected with feed liquor house steward；
B, liquid separation mechanism includes several triple valves, and each triple valve includes an inlet and two liquid outlets；It is flowed with liquid
Direction is downstream direction, and the inlet positioned at the triple valve of most upstream is connected with feed liquor house steward, and vertically roam all around the would is to being connected
Triple valve in, the inlet of two triple valves of two liquid outlets and opposite downstream of a triple valve of upstream relative is one by one
Corresponding connection；The total quantity of the liquid outlet of each triple valve of most downstream is identical as the quantity of analytical column and corresponds connection.
The invention also discloses integrate the method that liquid chromatogram column device carries out liquid phase preparation, preparation using above-mentioned multichannel
The process of liquid phase is: sample with mobile phase by feed liquor house steward and liquid separation mechanism even into each analytical column, each separation component with
Mobile phase is successively in charge of each analytical column of outflow by going out liquid, eventually enters into collection vessel, will be different by replacement collection vessel
The separation component of time outflow is collected in different collection vessels；
During above-mentioned preparation liquid phase, the intracorporal temperature of case is maintained at by predetermined temperature section, constant temperature by constant temperature method
Method is:
Electric control gear opens electric fan, and electric fan forms airflow circulating in cabinet, and air-flow makes the temperature in cabinet everywhere more
Uniformly, the even heat for generating electric heating tube each analytical column is heated；
TM DEG C of target temperature is stored in electric control gear；Electric control gear receives the temperature signal that temperature sensor detects, temperature
The actual temperature for the box house that sensor detects is TS DEG C；As TS < TM-2, electric control gear, which controls electric heating tube, to be continued
Electrified regulation；As (TM-2)≤TS < (TM-1), electric control gear, which controls the every work of electric heating tube 2 seconds, stops 1 second；When
(TM-1)≤TS < TM when, every work 2 seconds stop 2 seconds；As TS=TM, electric control gear controls the every work 2 of electric heating tube
Second stop 3-5 seconds；As (TM+1) > TS > TM, electric control gear keeps the working condition of electric heating tube constant；As (TM+
1)≤TS when, electric control gear close electric heating tube.
Multichannel of the invention integrates liquid chromatogram column device and multiple analytical columns is connected in parallel on one by structures such as multiple-way valves
It rises, improves total sample treatment ability, combine analytical column good separating effect and prepare the big advantage of column sample volume, overcome
The defect that analytical column sample volume is small and preparation post separation effect is poor, first separation can be equivalent to original separating for several times operation,
Use that is efficient and facilitating chromatographic column, energy first separation go out a variety of desired compounds, save the separation costs of complex compound,
This detection for arriving national sector greatly, medicine preparation (reduces medicine preparation cost, reduces medicine valence), small to arrive living environment, all
It makes great sense.
There is air interlayer between double transparent material, not only improved the thermal insulation property of chamber door, but also is logical convenient for operator
Cross the working condition that chamber door observes each analytical column.
On the one hand metal perforated plate plays the role of facilitating stationary chromatographic column, one side metal perforated plate plays Homogeneouslly-radiating work again
With, keep the temperature in cabinet everywhere more uniform using the good heating conduction of metal, porous structure is conducive to the circulation of air,
Air-flow caused by electric fan is by the spatial flow outside aperture and two metal perforated plates, the even heat that electric heating tube is generated
Ground is dispersed into cabinet space everywhere.
Liquid separation mechanism structure is simple, uniform with liquid, and the component used such as pipeline, multiple-way valve and triple valve etc. are experiment
Room common part, maintenance and replacement are very convenient.
Using the present invention carry out liquid phase preparation method, box house actual temperature distance objective temperature farther out when,
Make electric heating tube full speed operation to improve the temperature of box house rapidly；Target temperature is risen in the actual temperature of box house
When near degree, the opening time of electric heating tube is gradually decreased to reduce the intracorporal temperature rise speed of case, prevents temperature rise too fast and makes
The intracorporal temperature of case is excessively high, on the one hand avoids energy dissipation, controls the intracorporal temperature of case preferably in target temperature
Near degree.When the intracorporal actual temperature of case is identical as target temperature, the electric heating tube opening time is shorter, it is easier to dissipate with cabinet
The speed of calorific value matches, and the intracorporal temperature change of case is slower, good constant-temperature effect.
When the intracorporal actual temperature of case is higher than 1 DEG C of target temperature or more, electric heating tube is completely closed, at this time electric heating tube
Waste heat and cabinet in the intracorporal temperature of case can be made to be maintained at target temperature in a long time higher than the heat of target temperature
Near degree, therefore before the intracorporal actual temperature TS of case drops to TM, do not need to open electric heating tube.
In short, the method for carry out liquid phase preparation of the invention can make the intracorporal temperature of case near target temperature when variation
Slowly, and in the intracorporal temperature of case variation is very fast (quickly heating or fast cooling) when far from target temperature, reduces energy
Waste, improves constant temperature effect.
The present invention can change the type of analytical column according to the difference of required separate substance chemical property, to reach separation
The purpose of product；For the demand for meeting different preparation amounts, the quantity of analytical column can be increased；The configuration of the present invention is simple helps
In large batch of production and extensive popularization and application.Multichannel integrates liquid chromatogram column device in laboratory and scientific research field
Liquid phase is prepared with important influence, clearly demarcated for the raising ten for isolating and purifying upper benefit of effective ingredient and natural products
Aobvious, selling market has a extensive future.
Detailed description of the invention
Fig. 1 is that multichannel integrates the structural schematic diagram of liquid chromatogram column device in the present invention after removing chamber door；
Fig. 2 is the left view schematic diagram that multichannel integrates liquid chromatogram column device after removing electric control gear and display screen；
Fig. 3 is electric control schematic diagram of the invention；
Fig. 4 is trifluoro uridine acid solution separating effect figure when preparing；
Fig. 5 is the analytical effect figure that multichannel integrates purified product obtained by each analytical column of liquid chromatogram column device；By upper in figure
Each wavy line under is respectively the analytical effect curve of purified product obtained by 1-4 analytical column；
Fig. 6 is that multichannel integrates purified product obtained by each analytical column of liquid chromatogram column device and prepares the analysis of column preparation solution
Comparison diagram.Four wavy lines in figure from top to bottom are respectively the analytical effect curve of purified product obtained by 1-4 analytical column；
A wavy line of bottom (i.e. Article 5 from top to bottom) is the analytical effect curve for preparing purified product obtained by column in figure.
Specific embodiment
As shown in Figures 1 to 6, multichannel of the invention integrates the cabinet 1 that liquid chromatogram column device includes front end opening, case
The coiling of 1 rear wall of body is provided with electric heating tube 2, and electric fan 3, the case in 3 front of electric fan are equipped in the cabinet 1 in 2 front of electric heating tube
Parallel interval is equipped with several analytical columns 4 in body 1, and 1 side wall of cabinet is hinged with chamber door in open-mouth, and chamber door includes doorframe 5 and is embedded in
Double transparent material 6 in doorframe 5 has cavity 7 between double transparent material 6；Transparent material is glass, it is preferred to use organic
Glass.
The top of each analytical column 4 is respectively connected with out liquid and is in charge of 8, and respectively liquid is in charge of and is collected for outlet tube beam 9, outlet tube beam 9 out
Pass-out cabinet, one in outlet tube beam 9 goes out liquid and is in charge of for connecting external liquid chromatogram detector, in outlet tube beam 9
Other liquid out are in charge of in the collection vessel 10 being passed through outside cabinet 1；Collection vessel 10 preferably uses receiving flask, liquid chromatogram detector
It is not shown for conventional equipment.
The bottom end of each analytical column 4 passes through liquid separation mechanism connection feed liquor house steward 11 respectively, and feed liquor house steward 11 stretches out 1 side wall of cabinet
And it is connected with the delivery pump of transport flow phase；Delivery pump is routine techniques, not shown.
Electric heating tube 2 and electric fan 3 are connected with an electric control gear 12, and electric control gear 12 is connected with display screen 13 and temperature
Sensor 14 is spent, electric control gear 12 and display screen 13 are respectively positioned on 1 outer wall of cabinet, and temperature sensor 14 is located inside cabinet 1.For
Keep temperature signal more accurate, multiple temperature sensors can be evenly arranged in cabinet, electric control gear takes each temperature sensor
Value of the uniform value as TS.TS is real number.
There is cavity 7 between double transparent material 6, not only improved the thermal insulation property of chamber door, but also pass through convenient for operator
Chamber door observes the working condition of each analytical column 4.
Electric control gear 12 is 86 computers or single-chip microcontroller, and PLC can also be used.
It is equipped with metal perforated plate 15 in cabinet 1 between the analytical column 4 and electric fan 3, is uniformly distributed on metal perforated plate 15
Have multiple apertures 16, metal perforated plate 15 is symmetrical above and below set there are two.The left and right ends of metal perforated plate 15 are fixedly connected on 1 side of cabinet
On wall.16 one side of aperture facilitates fixed screw, is screwed analytical column 4, on the other hand facilitates air pair in cabinet 1
Stream.
Analytical column spacing side by side is equipped with multiple, and any one of the liquid separation mechanism is using following two structure:
A, liquid separation mechanism includes multiple-way valve, and multiple-way valve has an inlet and a several liquid outlets, the liquid outlet of multiple-way valve with point
It analyses column and corresponds connection；The inlet of multiple-way valve is connected with feed liquor house steward；
B, liquid separation mechanism includes several triple valves, and each triple valve includes an inlet and two liquid outlets；It is flowed with liquid
Direction is downstream direction, and the inlet positioned at the triple valve of most upstream is connected with feed liquor house steward, and vertically roam all around the would is to being connected
Triple valve in, the inlet of two triple valves of two liquid outlets and opposite downstream of a triple valve of upstream relative is one by one
Corresponding connection；The total quantity of the liquid outlet of each triple valve of most downstream is identical as the quantity of analytical column and corresponds connection.
The first is simple for structure, compact, but needs using special multiple-way valve；Second of structure member quantity is more, even
Connect it is relative complex, but since natively there is triple valve in laboratory, have convenient for gathering materials on the spot, joint connection in site production it is excellent
Point.
In the present embodiment, there are four 4 spacing side by side of analytical column is set, the liquid separation mechanism uses second of structure, including total
The inlet of triple valve 17, total triple valve 17 connects feed liquor house steward 11, and two liquid outlets of total triple valve 17 are separately connected one
Inlet with liquid triple valve 18, each to have with liquid triple valve 18 there are two liquid outlet, two four for matching liquid triple valve 18 go out
Liquid mouth is connected to the inlet of four analytical columns 4 by the one-to-one correspondence of feed liquor branch pipe 19；
Liquid separation mechanism structure is simple, and uniform with liquid, component used such as pipeline, triple valve etc. is laboratory common part, dimension
Shield and replacement are very convenient.
The invention also discloses integrate the method that liquid chromatogram column device carries out liquid phase preparation using above-mentioned multichannel.
The process of preparation liquid phase is: sample is with mobile phase by feed liquor house steward 11 and liquid separation mechanism even into each analytical column
4, each separation component is successively in charge of each analytical column 4 of 8 outflows by going out liquid with mobile phase, eventually enters into collection vessel 10, passes through
The separation component that replacement collection vessel 10 flows out different time is collected in different collection vessels 10；
During above-mentioned preparation liquid phase, the temperature in cabinet 1 is maintained at by predetermined temperature section, constant temperature by constant temperature method
Method is:
Electric control gear 12 opens electric fan 3, and electric fan 3 forms airflow circulating in cabinet 1, and air-flow makes the temperature in cabinet 1 everywhere
Heat each analytical column 4 with spending more uniform, to generate electric heating tube 2 even heat；
TM DEG C of target temperature is stored in electric control gear 12, TM is real number.Electric control gear 12 receives temperature sensor 14 and detects
Temperature signal, the actual temperature inside cabinet 1 that temperature sensor 14 detects be TS DEG C；As TS < TM-2, automatically controlled dress
It sets 12 control electric heating tubes 2 and continues electrified regulation；As (TM-2)≤TS < (TM-1), electric control gear 12 controls electric heating tube
2 every work 2 seconds stop 1 second；As (TM-1)≤TS < TM, stop 2 seconds within every work 2 seconds；As TS=TM, electricity
It controls device 12 and controls and stop within 2 every work of electric heating tube 2 seconds that (specific value was according to the integral heat sink speed of cabinet 1 in 3-5 seconds
Depending on, the heat dissipation of cabinet 1 is faster, then the dwell time of electric heating tube 2 is shorter)；As (TM+1) > TS > TM, electric control gear 12 is protected
The working condition for holding electric heating tube 2 is constant (in this temperature range, 2 every work of electric heating tube 2 seconds when generally in the temperature rising stage
Clock stops 3-5 seconds；Electric heating tube 2 stops working when declining the phase generally in temperature, until TS=TM)；As (TM+1)≤TS
When, electric control gear 12 closes electric heating tube 2.
Using constant temperature method of the invention, the actual temperature distance objective temperature inside cabinet 1 farther out when, make electric heating
2 full speed operation of pipe is to improve rapidly the temperature inside cabinet 1；It is attached that actual temperature inside cabinet 1 rises to target temperature
When close, the opening time of electric heating tube 2 is gradually decreased to reduce the temperature rise speed in cabinet 1, prevents temperature rise too fast and makes case
Temperature in body 1 is excessively high, on the one hand avoids energy dissipation, controls the temperature in cabinet 1 preferably in target temperature
Near degree.When the actual temperature in cabinet 1 is identical as target temperature, 2 opening time of electric heating tube is shorter, it is easier to cabinet
1 speed for distributing heat matches, and the temperature change in cabinet 1 is slower, good constant-temperature effect.
When the actual temperature in cabinet 1 is higher than 1 DEG C of target temperature or more, electric heating tube 2 is completely closed, at this time electric heating
Heat in the waste heat and cabinet 1 of pipe 2 higher than target temperature can make the temperature in cabinet 1 be maintained at mesh in a long time
It marks near temperature, therefore before the actual temperature TS in cabinet 1 drops to TM, does not need to open electric heating tube 2.
In short, the method for carry out liquid phase preparation of the invention can make the time-varying near target temperature of the temperature in cabinet 1
Change slowly, and variation when far from target temperature of the temperature in cabinet 1 is very fast (quickly heating or fast cooling), reduces energy
Amount waste, improves constant temperature effect.
The validity of liquid chromatogram column device is integrated for verifying multichannel, inventor is tested.
Experimental program:
(1) trifluoro uridine acid solution to be separated is configured, integrates liquid chromatogram column device using multichannel of the invention
Solution is separated, separating effect mirror then is carried out to purified product obtained by every analytical column in the present invention using analytical column
It is fixed.
(2) use prepares column and separates to same amount of trifluoro uridine acid solution, and using analytical column to system
Standby liquid carries out separating effect identification.
Trifluoro uridine acid solution separating effect is as shown in Figure 4 when preparation.
Four analytical columns 4 that multichannel integrates liquid chromatogram column device are compiled respectively as 1-4 analytical column.No. 1-4 analysis
The analysis chart of column is as shown in Figure 5.
It is analyzed as integrating purified product obtained by liquid chromatogram column device to multichannel, we can be found that every
4 good separation of analytical column and separating effect is almost the same (as shown in Figure 5).Liquid-phase chromatographic column is integrated by comparison multichannel
Device separating effect and preparation post separation effect, we can be found that under conditions of smaller sample volume, multichannel of the invention
The method that integrated liquid chromatogram column device carries out liquid phase preparation, can reach preparation solution phase effect same as column is prepared, illustrate
Feasibility of the device in preparation liquid phase.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although referring to above-described embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that: still the present invention can be modified or be waited
With replacement, without departing from the spirit or scope of the invention, or any substitutions, should all cover in power of the invention
In sharp claimed range.
Claims (4)
1. multichannel integrates liquid chromatogram column device, it is characterised in that: the cabinet including front end opening, the coiling setting of cabinet rear wall
There is electric heating tube, electric fan is equipped in the cabinet in front of electric heating tube, parallel interval is equipped with several in the cabinet in front of electric fan
Analytical column, wall box are hinged with chamber door in open-mouth, and chamber door includes doorframe and the double transparent material in doorframe, bilayer
There is cavity between transparent material；
The top of each analytical column is respectively connected with out liquid and is in charge of, and respectively liquid is in charge of and is collected for outlet tube beam out, outlet tube beam pass-out cabinet,
One in outlet tube beam goes out liquid and is in charge of for connecting external liquid chromatogram detector, and other liquid out in outlet tube beam are in charge of
It is passed through in the collection vessel outside cabinet；
The bottom end of each analytical column passes through liquid separation mechanism connection feed liquor house steward respectively, and feed liquor house steward stretches out wall box and and transport Stream
The delivery pump of dynamic phase is connected；
Electric heating tube and electric fan are connected with an electric control gear, and electric control gear is connected with display screen and temperature sensor, electricity
Control device and display screen are respectively positioned on cabinet exterior, and temperature sensor is located in the box body portion.
2. multichannel according to claim 1 integrates liquid chromatogram column device, it is characterised in that: the analytical column and electric wind
It is equipped with metal perforated plate in cabinet between fan, is evenly distributed with multiple apertures on metal perforated plate, metal perforated plate is symmetrical above and below to be equipped with
Two.
3. multichannel according to claim 1 integrates liquid chromatogram column device, it is characterised in that: analytical column spacing side by side is set
Have multiple, any one of the liquid separation mechanism is using following two structure:
A, liquid separation mechanism includes multiple-way valve, and multiple-way valve has an inlet and a several liquid outlets, the liquid outlet of multiple-way valve with point
It analyses column and corresponds connection；The inlet of multiple-way valve is connected with feed liquor house steward；
B, liquid separation mechanism includes several triple valves, and each triple valve includes an inlet and two liquid outlets；It is flowed with liquid
Direction is downstream direction, and the inlet positioned at the triple valve of most upstream is connected with feed liquor house steward, and vertically roam all around the would is to being connected
Triple valve in, the inlet of two triple valves of two liquid outlets and opposite downstream of a triple valve of upstream relative is one by one
Corresponding connection；The total quantity of the liquid outlet of each triple valve of most downstream is identical as the quantity of analytical column and corresponds connection.
4. integrating the method that liquid chromatogram column device carries out liquid phase preparation using multichannel as claimed in claim 2, feature exists
In:
The process of preparation liquid phase is: sample with mobile phase by feed liquor house steward and liquid separation mechanism even into each analytical column, each point
Successively it is in charge of each analytical column of outflow by going out liquid with mobile phase from component, eventually enters into collection vessel, collected and held by replacement
The separation component that device flows out different time is collected in different collection vessels；
During above-mentioned preparation liquid phase, the intracorporal temperature of case is maintained at by predetermined temperature section, constant temperature by constant temperature method
Method is:
Electric control gear opens electric fan, and electric fan forms airflow circulating in cabinet, and air-flow makes the temperature in cabinet everywhere more
Uniformly, the even heat for generating electric heating tube each analytical column is heated；
TM DEG C of target temperature is stored in electric control gear；Electric control gear receives the temperature signal that temperature sensor detects, temperature
The actual temperature for the box house that sensor detects is TS DEG C；As TS < TM-2, electric control gear, which controls electric heating tube, to be continued
Electrified regulation；As (TM-2)≤TS < (TM-1), electric control gear, which controls the every work of electric heating tube 2 seconds, stops 1 second；When
(TM-1)≤TS < TM when, every work 2 seconds stop 2 seconds；As TS=TM, electric control gear controls the every work 2 of electric heating tube
Second stop 3-5 seconds；As (TM+1) > TS > TM, electric control gear keeps the working condition of electric heating tube constant；As (TM+
1)≤TS when, electric control gear close electric heating tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910393885.9A CN110018264A (en) | 2019-05-13 | 2019-05-13 | The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910393885.9A CN110018264A (en) | 2019-05-13 | 2019-05-13 | The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation |
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|---|---|
| CN110018264A true CN110018264A (en) | 2019-07-16 |
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ID=67193549
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| CN201910393885.9A Pending CN110018264A (en) | 2019-05-13 | 2019-05-13 | The method that multichannel integrates liquid chromatogram column device and carries out liquid phase preparation |
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