CN106885781A - A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate - Google Patents
A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate Download PDFInfo
- Publication number
- CN106885781A CN106885781A CN201710206516.5A CN201710206516A CN106885781A CN 106885781 A CN106885781 A CN 106885781A CN 201710206516 A CN201710206516 A CN 201710206516A CN 106885781 A CN106885781 A CN 106885781A
- Authority
- CN
- China
- Prior art keywords
- ultraviolet
- flow cell
- pipe
- group
- uviol lamps
- 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.)
- Pending
Links
- 238000004440 column chromatography Methods 0.000 title claims abstract description 15
- 230000009977 dual effect Effects 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000005070 sampling Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims description 10
- 230000003321 amplification Effects 0.000 claims description 9
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims 1
- 229940058401 polytetrafluoroethylene Drugs 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 12
- 150000001875 compounds Chemical class 0.000 description 9
- 238000000034 method Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 238000004809 thin layer chromatography Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention discloses a kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate, it is characterised in that including sampling system, light-source system, data handling system；Described sampling system is made up of polyfluortetraethylene pipe and flow cell, and the polyfluortetraethylene pipe is connected with the flow cell, and sample liquid flows through flow cell by polyfluortetraethylene pipe；Described light-source system is made up of 365nm uviol lamps, 254nm uviol lamps, rectifier and transformer；The data handling system is by the first Ultraviolet sensor, the second Ultraviolet sensor, 8 single-chip microcomputers, the first group of four figures pipe, the second group of four figures pipe and serial data wire terminal, host computer composition；The present invention has relative low price, and safety is practical, easy to operate, the features such as, having promote well and practical value, and good economic and social benefit can be produced after extensive promotion and application.
Description
Technical field
It is more particularly to a kind of for normal the present invention relates to one kind for ultraviolet rapid detection apparatus during column chromatography for separation
The ultraviolet dual wave-band fast detector that pressure, medium pressure column chromatography are separate.
Background technology
In the extracting and developing and purge process of organic synthesis and natural drug, column chromatography for separation is using the most
Universal and extensive separation and purification technique.And its detection typically uses manual method：First launched with thin-layer chromatography, then with purple
Outer analysis instrument is observed, or is observed with uv analyzer again after sprinkling developer.
The method exist problem be：1. workload is big, and every batch of sample is required for detection；2. detection sensitivity is than relatively low：
In process of the test, thin-layer chromatography detection method needs to merge the intersection for so resulting in compound to the sample liquid collected, and makes
Obtaining the compound for being able to separate originally will carry out secondary separation, thus significantly increase the cumbersome and difficulty of experimentation,
And further loss will be caused to separator；3. thin layer detection can not with experiment synchronously carry out, there is certain hysteresis quality,
Expansion detection is carried out after needing sampling, and duration of run is long, it is difficult to realize to testing and producing efficient requirement.Especially
It is that pressure column chromatography is not difficult to carry out liquid stream a small amount of multiple collection in the middle pressure separation process of natural products, typically,
This allows for be detected using thin-layer chromatography in a large amount of preparation process, can only carry out it is without basis beat section, then divided again
From, may so cause script initial gross separation compound intersect it is serious.
Ultraviolet Detector of the prior art uses single band measuring method (CN 2553374Y), the light warp that light source sends
Form monochromatic light after crossing optical filter, by after sample cell with sample effect, be partly absorbed by the sample, partly through flow cell, shine
Electrooptical device is mapped to, electric signal is converted to, will be simulated by D/A converter module again after amplifying circuit amplifies signal
Signal is converted to the data signal proportional with concentration.Curve is drawn out through numeral method or output to specific register instrument
Figure, then carry out later stage treatment.
But, the complex structure of compound, species is various, and the wave band of its UV absorption is also incomplete same, only with
The compound that other do not possess wave band absorption is inevitably omitted in the absorption of single wave band detection compound.Some single ripples
Although the UV-detector of section can select 2 wave bands, compound cannot be monitored using 2 wave bands simultaneously, lost
Leakage is still inevitable.Meanwhile, instrument directly can not be connected with computer, it is necessary to a recorder record data.Instrument is heavy, operation
Trouble.
The content of the invention
Quickly examined it is an object of the invention to provide a kind of ultraviolet dual wave-band for for normal pressure, medium pressure column chromatography separate is provided
Instrument is surveyed, wavelength that can be simultaneously to 254nm and 365nm wave bands is detected, greatly extends the detection model of different compounds
Enclose, by upper computer software, more directly perceived will accurately grasp column chromatography for separation situation, can be with by observing real-time absorption curve
More intuitively grasp the separation situation of compound.
To achieve the above object, technical scheme is as follows：
A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate, including sampling system, light source system
System, data handling system；Described sampling system is made up of polyfluortetraethylene pipe and flow cell, the polyfluortetraethylene pipe and institute
State flow cell to be connected, sample liquid flows through flow cell by polyfluortetraethylene pipe；Described light-source system is by 365nm uviol lamps, 254nm
Uviol lamp, rectifier and transformer composition；The data handling system is by the first Ultraviolet sensor, the second Ultraviolet sensor, 8
Position single-chip microcomputer, the first group of four figures pipe, the second group of four figures pipe and serial data wire terminal, host computer composition；The circulation
The side in pond is provided with the 365nm uviol lamps and 254nm uviol lamps, opposite side and the 365nm uviol lamps and 254nm uviol lamps
Corresponding position is provided with the first Ultraviolet sensor and the second Ultraviolet sensor, first Ultraviolet sensor and the second ultraviolet biography
Sensor is connected with 8 single-chip microcomputers；8 single-chip microcomputers respectively with the first group of four figures pipe, the second group of four figures pipe phase
Even；8 single-chip microcomputers are connected by serial data wire terminal with the host computer.
Preferably, the ultraviolet dual wave-band fast detector also includes amplification module and analog-to-digital converting module, described
First Ultraviolet sensor and the second Ultraviolet sensor are connected with an amplification module respectively, and the amplification module passes through a mould respectively
Plan/data-converting block is connected with 8 single-chip microcomputers.
Compared with prior art, the device have the advantages that：During sample liquid flows through flow cell, by monolithic
Machine not only transmits the display of light absorption value, and send one to serial ports while different-waveband Ultraviolet sensor is read to charactron
The two-parameter data of group, after host computer receives, can change with time and draw out the photon absorbing intensity of two waveband.So achieve that
To the line real time monitoring and analyzing of efflux.The present invention has relative low price, and safety is practical, easy to operate, the features such as,
Having promote well and practical value, and good economic and social benefit can be produced after extensive promotion and application.
Brief description of the drawings
Fig. 1 is structural representation of the invention
Fig. 2 is operational module structural representation of the present invention
Fig. 3 is testing result oscillogram of the present invention
Wherein, 1- rectifiers, 2- polyfluortetraethylene pipes, 3- flow cells, 4- first group of four figures pipes, the groups of four figures of 5- second
Pipe, the Ultraviolet sensors of 6- first, 7-254nm uviol lamps, the Ultraviolet sensors of 8- second, 9-365nm uviol lamps, 10- transformers,
11-8 single-chip microcomputer, 12- serial data wire terminals.
Specific embodiment
The technical scheme to this patent is described in more detail below in conjunction with the accompanying drawings.
A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate, including sampling system, light source system
System, data handling system；Described sampling system is made up of polyfluortetraethylene pipe 2 and flow cell 3, the polyfluortetraethylene pipe 2
It is connected with the flow cell 3, sample liquid flows through flow cell 3 by polyfluortetraethylene pipe 2；Described light-source system is ultraviolet by 365nm
Lamp 9,254nm uviol lamps 7, rectifier 1 and transformer 10 are constituted；The data handling system is by the first Ultraviolet sensor 6,
Two single-chip microcomputers 11 of Ultraviolet sensor 8,8, the first group of four figures pipe 4, the second group of four figures pipe 5 and serial data wire terminal
12nd, host computer composition；The side of the flow cell 3 is provided with the 365nm uviol lamps 9 and 254nm uviol lamps 7, opposite side and institute
State 365nm uviol lamps 9 and the corresponding position of 254nm uviol lamps 7 be provided with the first Ultraviolet sensor 6 and the second Ultraviolet sensor 8,
The Ultraviolet sensor 8 of first Ultraviolet sensor 6 and second is connected with 8 single-chip microcomputers 11；11 points of 8 single-chip microcomputers
It is not connected with the first group of four figures pipe 4, the second group of four figures pipe 5；8 single-chip microcomputers 11 by serial data wire terminal 12 with
The host computer connection.
Meanwhile, in order that the detection of this instrument is more precisely, and also including amplification module and analog-to-digital converting module, described the
One Ultraviolet sensor 4 and the second Ultraviolet sensor 5 are connected with an amplification module respectively, and the amplification module passes through a mould respectively
Plan/data-converting block is connected with 8 single-chip microcomputers 11.
Detection experiment：
In under normal pressure, sample 1 is separated：Ethyl (E) -3-4- fluorobenzene base esters, sample 2：The tert-butyl group (E) -3- (2- hydroxyls -3-
Methoxyl group) acrylate, chromatographic column is silicagel column, and filler is 100 mesh, and applied sample amount is 200mg；
Prior to installing inspection software in calculating, and install after CH340 drives, by USB line by computer and ultraviolet detection
Instrument is connected；Now, the first charactron 4 is shown as " BULB ", represents that uviol lamp is closed；Instrument is accessed into column chromatography system
After uniting and ensureing that liquid stream flows through instrument, column chromatography valve is closed, open instrument and simultaneously switch.Now, the charactron of instrument first shows
It is shown as " CHEC ", represents that instrument carries out ultraviolet calibration.Current light absorption value is shown when calibrating and completing, while clicking on computer
Software carries out serial ports scanning.After obtaining Serial Port Information, it is the real-time monitoring for being capable of achieving computer software to click on and open serial ports.
Detection and analysis result such as 3,8 single-chip microcomputers 11 of accompanying drawing send data to computer software by serial ports, to double ginsengs
Number carries out hyperbola drawing, while detecting ethyl (E) -3-4- fluorobenzene base ester and the tert-butyl group (E) -3- (2- hydroxyl -3- methoxies
Base) acrylate.
Above-listed detailed description is directed to illustrating for possible embodiments of the present invention, and the embodiment simultaneously is not used to limit this hair
Bright the scope of the claims, all equivalence enforcements or change without departing from carried out by the present invention are intended to be limited solely by the scope of the claims of this case.
Claims (2)
1. it is a kind of for normal pressure, the ultraviolet dual wave-band fast detector of medium pressure column chromatography separation, it is characterised in that including sample introduction system
System, light-source system, data handling system；Described sampling system is made up of polyfluortetraethylene pipe and flow cell, the polytetrafluoro
Ethylene tube is connected with the flow cell, and sample liquid flows through flow cell by polyfluortetraethylene pipe；Described light-source system is purple by 365nm
Outer lamp, 254nm uviol lamps, rectifier and transformer composition；The data handling system is by the first Ultraviolet sensor, the second purple
Outer sensor, 8 single-chip microcomputers, the first group of four figures pipe, the second group of four figures pipe and serial data wire terminal, upper unit
Into；The side of the flow cell is provided with the 365nm uviol lamps and 254nm uviol lamps, opposite side and the 365nm uviol lamps and
The corresponding position of 254nm uviol lamps is provided with the first Ultraviolet sensor and the second Ultraviolet sensor, first Ultraviolet sensor
It is connected with 8 single-chip microcomputers with the second Ultraviolet sensor；8 single-chip microcomputers respectively with the first group of four figures pipe, second
Group of four figures pipe is connected；8 single-chip microcomputers are connected by serial data wire terminal with the host computer.
2. according to claim 1 for normal pressure, the ultraviolet dual wave-band fast detector of medium pressure column chromatography separation, its feature
It is that the ultraviolet dual wave-band fast detector also includes amplification module and analog-to-digital converting module, the first ultraviolet biography
Sensor and the second Ultraviolet sensor are connected with an amplification module respectively, and the amplification module passes through an analog/digital conversion respectively
Module is connected with 8 single-chip microcomputers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710206516.5A CN106885781A (en) | 2017-03-31 | 2017-03-31 | A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710206516.5A CN106885781A (en) | 2017-03-31 | 2017-03-31 | A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106885781A true CN106885781A (en) | 2017-06-23 |
Family
ID=59182682
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710206516.5A Pending CN106885781A (en) | 2017-03-31 | 2017-03-31 | A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106885781A (en) |
-
2017
- 2017-03-31 CN CN201710206516.5A patent/CN106885781A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN207516315U (en) | Non-methane total hydrocarbons detection device | |
| CN202916200U (en) | Medical fluorescent quantitation analysis meter | |
| CN1979172B (en) | Gas analyzing method | |
| CN107643352A (en) | NMHC detection means and method | |
| CN203941099U (en) | Gas phase molecular absorption spectrometer with on-line oxidation device | |
| CN112834572B (en) | Gas sensor testing method applied to detection of sulfur hexafluoride and decomposition product gas sensor thereof | |
| CN206601333U (en) | A kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography | |
| CN204128960U (en) | A kind of drinks quality sense organ classification quick analytic instrument | |
| CN201449370U (en) | Multi-wavelength nucleic acid protein chromatographic separation detection device | |
| CN100559353C (en) | Method for detecting rapidly computer hardware equipment function completeness | |
| CN102393393A (en) | Detection device and detection method for content of heavy metal in foods | |
| CN106885781A (en) | A kind of ultraviolet dual wave-band fast detector for for normal pressure, medium pressure column chromatography separate | |
| CN101144779A (en) | Dark current detection device and absorbency detection method | |
| CN106501430A (en) | The detection method of the volatile organic matter related to pulmonary carcinoma in a kind of respiratory gass | |
| CN207366571U (en) | A kind of gold mark and fluorescence immune chromatography synthesis analyzer | |
| CN110763774A (en) | Device and method for testing hydrogen evolution and absorption performance of ointment | |
| CN1458529A (en) | Colorimetric component analysis method and its device based on image technology | |
| CN101620182A (en) | Multi-wavelength nucleic acid protein chromatographic separation detecting system | |
| CN104502481A (en) | Method for detecting vomitoxin and zearalenone in grains and feeds | |
| CN207248730U (en) | A kind of blood urine measures Biochemical Analyzer | |
| CN106680267A (en) | Quantitative analysis system for urine iodine | |
| CN201464441U (en) | Digital UV detector | |
| CN203786025U (en) | On-line detection device for pesticide concentrations | |
| CN206248539U (en) | Quantitative analysis instrument | |
| CN1136448C (en) | Selective poison gas alarm and alarm method |
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 |