CN102565255A - PCEC (Pressurized Capillary Electrochromatography) ELSD (Evaporative Light-Scattering Detector) - Google Patents
PCEC (Pressurized Capillary Electrochromatography) ELSD (Evaporative Light-Scattering Detector) Download PDFInfo
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- CN102565255A CN102565255A CN2011101379327A CN201110137932A CN102565255A CN 102565255 A CN102565255 A CN 102565255A CN 2011101379327 A CN2011101379327 A CN 2011101379327A CN 201110137932 A CN201110137932 A CN 201110137932A CN 102565255 A CN102565255 A CN 102565255A
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Abstract
The invention discloses a PCEC (Pressurized Capillary Electrochromatography) ELSD (Evaporative Light-Scattering Detector). The PCEC ELSD is composed by connecting a PCEC and an ELSD, wherein an atomized capillary tube is inserted in a center hole of an atomizer of the ELSD, the front end of the atomized capillary tube is connected with a capillary chromatographic column in the PCEC through an electric isolation device, and the distance between the tail end of the atomized capillary tube and an outlet of the center hole of the atomizer is 0mm-0.5mm. The PCEC ELSD disclosed by the invention is compatible with the advantages of high column effect, high selectivity, high resolution and quick separation of the PCEC and the advantage of generality of the ELSD, thus the PCEC ELSD can be used for separating and detecting substances without a functional group of ultraviolet and fluorescence characteristics and has an extremely wide application prospect particularly in the fields of analyzing natural products (comprising Chinese medicinal herbs), medicines and food and the like.
Description
Technical field
The present invention relates to a kind of chemical analysis instrument, be specifically related to a kind of pressurization capillary electric chromatogram evaporative light-scattering pick-up unit.
Background technology
Pressurization capillary electric chromatogram (Pressurized Capillary electrochromatography; PCEC) be Capillary Electrophoresis (Capillary electrophoresis; CE) technology and high performance liquid chromatography (High Performance Liquid Chromatography; HPLC) combination of technology has the dual separating mechanism of Capillary Electrophoresis and high performance liquid chromatography concurrently, is that a kind of novel efficient differential is from technology.Compare with high performance liquid chromatography with the Capillary Electrophoresis of transmission system; Pressurization capillary electric chromatogram is separating charged substance and neutral substance simultaneously; Reduced the peak broadening in the chromatographic separation process widely; Have Gao Zhuxiao, high selectivity, high resolving power, quick characteristics of separating, all obtained using widely in fields such as life science, traditional Chinese medicine research, Pharmaceutical Analysis, environmental protection, food security, chemicals.Pressurization capillary electric chromatogram mainly contains detection meanss such as ultraviolet absorption method, laser inductive fluorescence method, electrochemical assay, mass spectroscopy and nuclear magnetic resonance at present.Wherein uv absorption and laser-Induced Fluorescence Detection method are the characteristic detection means, and the material that only has ultraviolet or fluorescence functional group just can be to be detected, and most material itself does not have uv absorption or fluorescence signal; Electrochemical Detection sensitivity is higher; Shortcoming is only to be suitable for detecting electroactive material or some non-electroactive materials of derivatization mensuration; In the commercialization process, need to solve such as a series of problems such as high-voltage electric field isolation, the accurate location of electrode, its range of application and application are restricted; And mass spectrum and magnetic resonance detection, instrument operation and maintenance cost is high, operates loaded down with trivial details.Therefore, the detection versatility of pressurization capillary electric chromatogram is not strong.
EISD (Evaporative light-scattering detector; ELSD); It is a kind of universal mass detector that the nineties begins to be used widely from last century; Compare the maximum UV-detector of use in the present liquid chromatographic detection, ELSD has higher versatility, does not receive the restriction of this body structure of material; Be applicable to the analyzing and testing of most non-volatile and half volatile substances, especially have more advantage in natural products (comprising Chinese herbal medicine), medicine, agricultural residual and food analysis fields such as (amino acid, carbohydrate, ester classes).
Summary of the invention
Technical matters to be solved by this invention provides a kind of pressurization capillary electric chromatogram EISD; This pressurization capillary electric chromatogram EISD has Gao Zhuxiao, high selectivity, high resolving power, the advantage of separating fast and the versatility advantage of EISD of pressurization capillary electric chromatogram concurrently, to overcome the deficiency that prior art exists.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of pressurization capillary electric chromatogram EISD; It is characterized in that: connect and compose by pressurization capillary electric chromatogram and EISD; Be inserted with the atomizing kapillary in the center pit of the atomizer of said EISD; This front end capillaceous that atomizes is connected with capillary chromatographic column in the pressurization capillary electric chromatogram through electric spacer assembly, and the distance that center pit terminal and atomizer exports is 0-0.5mm.
Outlet indentation certain distance in above-mentioned scope at atomizing end capillaceous and atomizer center pit described in the preferred implementation of the present invention is good.
In embodiment of the present invention, said atomizing external diameter capillaceous is slightly less than the aperture of atomizer center pit, and its value scope is at 150～360 μ m, and internal diameter is 10-100 μ m.
Said capillary chromatographic column can be open tubular column, a kind of in packed column or the integral post.
Said atomizing kapillary can be tapered, cylindrical, and material is a quartz capillary.
Said atomizing kapillary is fastened on the inflow point of atomizer center pit through the PEEK screw.
Adopt technique scheme; Through utilizing atomizing kapillary and electric spacer assembly that pressurization capillary electric chromatogram and EISD are coupled together pressurization capillary electric chromatogram EISD of formation; Thereby make pick-up unit of the present invention have the Gao Zhuxiao of pressurization capillary electric chromatogram, high selectivity, high resolving power, the advantage of separating fast and the versatility advantage of EISD concurrently; Make it can separation detection not have the material of ultraviolet and fluorescent characteristics functional group, especially have utmost point application prospects in fields such as natural products (comprising Chinese herbal medicine), medicine and food analyses.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is a detection collection of illustrative plates of the present invention.
Embodiment
Lift a preferred embodiment below, and combine accompanying drawing to come the clearer the present invention that intactly explains.
As shown in Figure 1, pressurization capillary electric chromatogram EISD of the present invention is connected and composed by pressurization capillary electric chromatogram 100 and EISD 15.
Pressurization capillary electric chromatogram 100 comprises that two are used to carry liquid flow phase high-pressure pump 2,3; Be used for the mixing valve 4 that the liquid flow phase gradient mixes; The four-way diverting valve 5 that is used for flow-dividing control, what be used for sample feeding receives upgrading sampling valve 6, is used to apply the backpressure valve 7 of buffer brake Control Flow; The capillary chromatographic column 8 that is used for sample separation is used for applying at the capillary chromatographic column two ends high-voltage power supply 10 of high-voltage electric field.
EISD 15 comprises the atomizer 12 that the liquid flow that connects is successively carried out gas atomization mutually, is used for the evaporation tube 13 of mobile phase solvent evaporation, is used for the light detection cell 14 that the sample particle scattering detects.
Wherein, One end of high-pressure pump 2,3 is communicated with a moving phase liquid storage bottle 1 respectively; The other end of high-pressure pump 2,3 is connecting on the mixing valve 4 again, and mixing valve 4 connects four-way diverting valve 5 again, and in addition three ports of four-way diverting valve 5 connect respectively receives upgrading sampling valve 6; The positive pole of backpressure valve 7 and high-voltage power supply 10, the upgrading sampling valve 6 of receiving connects separation capillary chromatographic column 8 again.
Pressurization capillary electric chromatogram 100 is connected with atomizing kapillary 11 through electric spacer assembly 9 with EISD 15.Particularly; Electricity spacer assembly 9 one ends connect separation capillary chromatographic column 8; One end connects the negative pole of high-voltage power supply 10; The other end connect to be gone up the front end of atomizing kapillary 11, and then in the center pit of insertion atomizer 12 and fastening with the PEEK screw in the inflow point of center pit, the distance that its center pit terminal and atomizer exports is 0-0.5mm to atomizing kapillary 11.
When concrete the application, separation capillary chromatographic column 8 can be open tubular column, a kind of in packed column or the integral post.The atomizing kapillary can be tapered, cylindrical, and material is a quartz capillary.
During use, EISD 15 is connected on the computing machine 16, and operation has the chromatogram workstation software on the computing machine 16.
More than be exactly pressurization capillary electric chromatogram EISD of the present invention, its course of work is following:
At first operation chromatographic work station software on computing machine 16 is provided with high-pressure pump 2,3, the running parameter of high-voltage power supply 10, EISD 15; Operation pressurization capillary electric chromatogram piece-rate system and evaporative light-scattering pick-up unit; The liquid flow high-pressure pump 2,3 that communicated is carried, and behind mixing valve 4,5 places shunt at the four-way diverting valve; Moving phase after the shunting is most of to flow into waste liquid through backpressure valve 7; Another part is received the upgrading flow and is pumped into separation capillary chromatographic column 8 through sampling valve 6, and sample can be separated from capillary chromatographic column 8 by the moving phase carry over score at sampling valve 6 place's sample introductions; Capillary chromatographic column 8 contain sample flow phase eluent, behind electric spacer assembly 9, link to each other with EISD 15 through atomizing kapillary 11; High-voltage power supply 10 applies electric field in shunting four-way valve 6 and electric spacer assembly 9 two ends through electrode, can in separation capillary chromatographic column 8, produce the EOF expulsive force, drives moving phase and carries out the electrochromatography separation; Electricity spacer assembly 9 has quarantine measures simultaneously as an end of electrode, and EISD 15 is isolated from outside the electric field, prevents that influence from detecting; The moving phase eluent that contains sample gets into atomizing kapillary 11; At the endpiece of atomizer 12, the effect through gas atomizes, and liquid mist changes into gasoloid; Under the conveying of gas, get into evaporation tube 13; Liquid flux is evaporated at evaporation tube 13, and remaining sample material particle gets into light detection cell 14 and carries out scattering and detection, and the scattered light signal of generation is converted into voltage signal through signal picker; And from the chromatographic work station software of computing machine 16, export, be the spectrogram that pressurization capillary electric chromatogram-evaporative light-scattering detects.
To detect 1.0 * 10
-3G/mL glucose, sucrose and lactose are example:
Experiment condition is: the capillary chromatographic column that the long 300 μ m internal diameters of 10cm are filled the amino filler of 5 μ m is as separation capillary chromatographic column 8; With 360 μ m external diameters, 50 μ m internal diameter quartz capillaries as the atomizing kapillary 11; Moving phase is that 80% acetonitrile (contains the 5mM ammonium acetate buffer; PH=7), separation voltage is 5kv, and flow rate pump is 0.05mL/min.Testing result is seen Fig. 2, and three chromatographic peaks are followed successively by 1. glucose, 2. sucrose, 3. lactose among Fig. 2.
Can find out that from test pressurization capillary electric chromatogram EISD of the present invention can detect glucose, sucrose and lactose, and from the collection of illustrative plates that detects, can find out that testing result has post effect, high selectivity, high-resolution characteristics.
In sum, the present invention has following advantage:
1. with Evaporative Light-Scattering Detection Technology and the coupling of pressurization capillary electric chromatogram isolation technics; With technical advantages such as pCEC Gao Zhuxiao, high selectivity, high resolving power, quick separation; " versatility " characteristic that detects with ELSD combines; Make it can separation detection not have the material of ultraviolet and fluorescent characteristics functional group, especially have utmost point application prospects in fields such as natural products (comprising Chinese herbal medicine), medicine and food analyses;
Evaporative Light-Scattering Detection Technology is microminiaturized 2., make it to go for receiving the upgrading separation system;
3. apparatus of the present invention are easy and simple to handle, and detection sensitivity is high, can realize the pressurization capillary electric chromatogram of non-volatile and half volatile material is separated and microminiaturized evaporative light-scattering detection.
Though more than described embodiment of the present invention, it will be understood by those of skill in the art that these only illustrate, under the prerequisite that does not deviate from principle of the present invention and essence, can make numerous variations or modification to these embodiments.Therefore, protection scope of the present invention is limited appended claims.
Claims (4)
1. pressurization capillary electric chromatogram EISD; It is characterized in that: connect and compose by pressurization capillary electric chromatogram and EISD; Be inserted with the atomizing kapillary in the center pit of the atomizer of said EISD; This front end capillaceous that atomizes is connected with capillary chromatographic column in the pressurization capillary electric chromatogram through electric spacer assembly, and the distance that center pit terminal and atomizer exports is 0-0.5mm.
2. pressurization capillary electric chromatogram EISD according to claim 1 is characterized in that: said atomizing external diameter capillaceous is slightly less than the aperture of atomizer center pit, and its value scope is at 150～360 μ m, and internal diameter is 10-100 μ m.
3. pressurization capillary electric chromatogram EISD according to claim 1 is characterized in that: said capillary chromatographic column can be open tubular column, a kind of in packed column or the integral post.
4. pressurization capillary electric chromatogram EISD according to claim 1 is characterized in that: said atomizing kapillary can be tapered, cylindrical, and material is a quartz capillary.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110137932.7A CN102565255B (en) | 2011-05-25 | 2011-05-25 | PCEC (Pressurized Capillary Electrochromatography) ELSD (Evaporative Light-Scattering Detector) |
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| CN201110137932.7A CN102565255B (en) | 2011-05-25 | 2011-05-25 | PCEC (Pressurized Capillary Electrochromatography) ELSD (Evaporative Light-Scattering Detector) |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103884814A (en) * | 2014-04-17 | 2014-06-25 | 厦门大学 | Ten-thousand-volt high-voltage electric field enhancement liquid chromatogram system |
| CN106680353A (en) * | 2017-03-21 | 2017-05-17 | 上海通微分析技术有限公司 | Electrochromatography device |
| CN109212145A (en) * | 2018-10-24 | 2019-01-15 | 东北师范大学 | A kind of novel high time resolution on-line checking drug-eluting process analysis method |
| CN110662958A (en) * | 2017-03-30 | 2020-01-07 | 九零八图案公司 | Microfluidic analysis of biological samples |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202083681U (en) * | 2011-05-25 | 2011-12-21 | 上海通微分析技术有限公司 | Pressurized capillary electrochromatography evaporative light scattering detector |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202083681U (en) * | 2011-05-25 | 2011-12-21 | 上海通微分析技术有限公司 | Pressurized capillary electrochromatography evaporative light scattering detector |
Non-Patent Citations (2)
| Title |
|---|
| JAMES N. ALEXANDER，IV: "Evaporative Light Scattering Detection for Microcolumn Liquid Chromatography", 《JOURNAL OF MICROCOLUMN SWPARATIONS》 * |
| 吴漪等: "毛细管电色谱和加压毛细管电色谱的进展与应用", 《色谱》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103884814A (en) * | 2014-04-17 | 2014-06-25 | 厦门大学 | Ten-thousand-volt high-voltage electric field enhancement liquid chromatogram system |
| CN103884814B (en) * | 2014-04-17 | 2015-10-14 | 厦门大学 | Ten thousand volts of high-voltage electric fields strengthen liquid chromatographic system |
| CN106680353A (en) * | 2017-03-21 | 2017-05-17 | 上海通微分析技术有限公司 | Electrochromatography device |
| CN110662958A (en) * | 2017-03-30 | 2020-01-07 | 九零八图案公司 | Microfluidic analysis of biological samples |
| CN110662958B (en) * | 2017-03-30 | 2023-03-07 | 九零八图案公司 | Microfluidic analysis of biological samples |
| CN109212145A (en) * | 2018-10-24 | 2019-01-15 | 东北师范大学 | A kind of novel high time resolution on-line checking drug-eluting process analysis method |
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