CN102565255B - 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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- CN102565255B CN102565255B CN201110137932.7A CN201110137932A CN102565255B CN 102565255 B CN102565255 B CN 102565255B CN 201110137932 A CN201110137932 A CN 201110137932A CN 102565255 B CN102565255 B CN 102565255B
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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 detector.
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, having the dual separating mechanism of Capillary Electrophoresis and high performance liquid chromatography concurrently, is a kind of novel efficient micro-isolation technics.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 widely the peak broadening in chromatographic separation process; there is Gao Zhuxiao, high selectivity, high resolving power, quick separated feature, in fields such as life science, traditional Chinese medicine research, Pharmaceutical Analysis, environmental protection, food security, chemicals, be all widely used.Pressurization capillary electric chromatogram mainly contains the 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 characteristic detection means, and the material only with ultraviolet or fluorescence functional group just can be detected, and most material itself there is no uv absorption or fluorescence signal; Electrochemical Detection sensitivity is higher, shortcoming is to be only suitable for detecting electroactive material or some non-electroactive materials of Derivatization Determination, in commercialization process, need to solve 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.
Evaporative light-scattering detector (Evaporative light-scattering detector, ELSD), it is a kind of universal mass detector that the nineties starts to be used widely from last century, compare and in current liquid chromatographic detection, use maximum UV-detector, ELSD has higher versatility, be not subject to the restriction of this body structure of material, be applicable to the analyzing and testing of most non-volatile and half volatile substances, especially at natural products (comprising Chinese herbal medicine), medicine, agriculture is residual and the field such as food analysis (amino acid, carbohydrate, ester class) has more advantage.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of pressurized capillary electrochromatographevaporative evaporative light scattering detector, this pressurized capillary electrochromatographevaporative evaporative light scattering detector has Gao Zhuxiao, high selectivity, high resolving power, the advantage of separation fast and the versatility advantage of evaporative light-scattering detector of pressurization capillary electric chromatogram, the deficiency existing to overcome prior art concurrently.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of pressurized capillary electrochromatographevaporative evaporative light scattering detector, it is characterized in that: by pressurization capillary electric chromatogram and evaporative light-scattering detector, connected and composed, in the center pit of the atomizer of described evaporative light-scattering detector, be inserted with atomization kapillary, this atomization front end capillaceous is connected with the capillary chromatographic column in pressurization capillary electric chromatogram by electric spacer assembly, and the distance of the center pit outlet of end and atomizer is 0-0.5mm.
Outlet indentation certain distance in above-mentioned scope at the end capillaceous of atomization described in the preferred embodiment of the present invention and atomizer center pit is good.
In the specific embodiment of the present invention, described atomization 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.
Described capillary chromatographic column can be open tubular column, a kind of in packed column or integral post.
Described atomization kapillary can be tapered, cylindrical, and material is quartz capillary.
Described atomization kapillary is the inflow point at atomizer center pit by PEEK screw fastening.
Adopt technique scheme, by utilizing atomization kapillary and electric spacer assembly that pressurization capillary electric chromatogram and evaporative light-scattering detector are coupled together and form a pressurized capillary electrochromatographevaporative evaporative light scattering detector, thereby make pick-up unit of the present invention have the Gao Zhuxiao of pressurization capillary electric chromatogram concurrently, high selectivity, high resolving power, quick separated advantage and the versatility advantage of evaporative light-scattering detector, make it separation to detect the material without ultraviolet and fluorescent characteristics functional group, especially at natural products (comprising Chinese herbal medicine), the field such as medicine and food analysis has utmost point application prospect widely.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is detection collection of illustrative plates of the present invention.
Embodiment
Lift a preferred embodiment below, and carry out by reference to the accompanying drawings the clearer the present invention that intactly illustrates.
As shown in Figure 1, pressurized capillary electrochromatographevaporative evaporative light scattering detector of the present invention, is connected and composed by pressurization capillary electric chromatogram 100 and evaporative light-scattering detector 15.
Pressurization capillary electric chromatogram 100 comprises that two for delivery of liquid flow phase high-pressure pump 2,3, the mixing valve 4 mixing for liquid flow phase gradient, four-way diverting valve 5 for flow-dividing control, the sampling valve 6 of upgrading of receiving for sample feeding, for applying buffer brake, control the backpressure valve 7 of flow, for the capillary chromatographic column 8 of sample separation, for apply the high-voltage power supply 10 of high-voltage electric field at capillary chromatographic column two ends.
Evaporative light-scattering detector 15 comprises the atomizer 12 that the liquid flow connecting is successively carried out to gas atomization mutually, for the evaporation tube 13 of mobile phase solvent evaporation, and the light detection cell 14 detecting for sample particle scattering.
Wherein, one end of high-pressure pump 2,3 is communicated with respectively a mobile phase liquid storage bottle 1, the other end of high-pressure pump 2,3 is connecting on mixing valve 4 again, mixing valve 4 connects four-way diverting valve 5 again, another three ports of four-way diverting valve 5 connect respectively receive 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 atomization kapillary 11 by electric spacer assembly 9 with evaporative light-scattering detector 15.Particularly, electricity spacer assembly 9 one end connect separation capillary chromatographic column 8, one end connects the negative pole of high-voltage power supply 10, the other end connects the front end of upper atomization kapillary 11, atomization kapillary 11 is in the center pit of insertion atomizer 12 and at inflow point's PEEK screw fastening of center pit, and the distance of the center pit outlet of its end and atomizer is 0-0.5mm.
When concrete application, separation capillary chromatographic column 8 can be open tubular column, a kind of in packed column or integral post.Atomization kapillary can be tapered, cylindrical, and material is quartz capillary.
During use, evaporative light-scattering detector 15 is connected on computing machine 16, and on computing machine 16, operation has chromatogram workstation software.
Be exactly more than pressurized capillary electrochromatographevaporative evaporative light scattering detector of the present invention, its course of work is as follows:
First on computing machine 16, move chromatographic work station software, high-pressure pump 2,3 is set, the running parameter of high-voltage power supply 10, evaporative light-scattering detector 15; Operation pressurization capillary electric chromatogram piece-rate system and evaporative light scattering detector, the liquid flow high-pressure pump 2,3 that communicated is carried, after mixing valve 4, at four-way diverting valve, 5 places shunt, mobile phase after shunting is most of through backpressure valve 7 inflow waste liquids, another part is received upgrading flow and is pumped into separation capillary chromatographic column 8 through sampling valve 6, and sample can, at sampling valve 6 place's sample introductions, be carried out separation by mobile phase carry over score from capillary chromatographic column 8; Capillary chromatographic column 8 containing sample flow phase eluent, after electric spacer assembly 9, by atomization kapillary 11, be connected with evaporative light-scattering detector 15; High-voltage power supply 10 applies electric field in dividing flow valve 6 and electric spacer assembly 9 two ends by electrode, can in separation capillary chromatographic column 8, produce electroosmotic flow expulsive force, drives mobile phase to carry out electrochromatography separation; Electricity spacer assembly 9, as one end of electrode, has quarantine measures simultaneously, and evaporative light-scattering detector 15 is isolated from outside electric field, prevents that electric field influence from detecting; Mobile phase eluent containing sample enters atomization kapillary 11, endpiece at atomizer 12, atomization is carried out in effect by gas, liquid mist changes into gasoloid, under the conveying of gas, enter evaporation tube 13, liquid flux is evaporated at evaporation tube 13, remaining sample material particle enters light detection cell 14 and carries out scattering and detection, the scattered light signal producing is converted into voltage signal through signal picker, and export from the chromatographic work station software of computing machine 16, 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, using 360 μ m external diameter 50 μ m internal diameter quartz capillaries as atomization kapillary 11, mobile phase is that 80% acetonitrile is (containing 5mM ammonium acetate buffer, pH=7), separation voltage is 5kv, and flow rate pump is 0.05mL/min.Testing result is shown in Fig. 2, and in Fig. 2, three chromatographic peaks are followed successively by 1. glucose 2. sucrose 3. lactose.
From test, can find out, pressurized capillary electrochromatographevaporative evaporative light scattering detector of the present invention can detect glucose, sucrose and lactose, and can find out from the collection of illustrative plates detecting, and testing result has post effect, high selectivity, high-resolution feature.
In sum, tool of the present invention has the following advantages:
1. by Evaporative Light-Scattering Detection Technology and the coupling of pressurization capillary electric chromatogram isolation technics, by technical advantages such as pCEC Gao Zhuxiao, high selectivity, high resolving power, quick separation, " versatility " feature detecting with ELSD combines, make it separation to detect the material without ultraviolet and fluorescent characteristics functional group, especially in fields such as natural products (comprising Chinese herbal medicine), medicine and food analyses, there is utmost point application prospect widely;
Evaporative Light-Scattering Detection Technology is microminiaturized 2., make it to go for receiving upgrading separation system;
3. apparatus of the present invention are easy and simple to handle, and detection sensitivity is high, can realize the separated and microminiaturized evaporative light-scattering of the pressurization capillary electric chromatogram of non-volatile and half volatile material is detected.
Although more than described the specific embodiment of the present invention, it will be understood by those of skill in the art that these only illustrate, do not deviating under the prerequisite of principle of the present invention and essence, can make various changes or modifications to these embodiments.Therefore, protection scope of the present invention is limited by appended claims.
Claims (3)
1. a pressurized capillary electrochromatographevaporative evaporative light scattering detector, it is characterized in that: by pressurization capillary electric chromatogram and evaporative light-scattering detector, connected and composed, in the center pit of the atomizer of described evaporative light-scattering detector, be inserted with atomization kapillary, this atomization front end capillaceous is connected with the capillary chromatographic column in pressurization capillary electric chromatogram by electric spacer assembly, and the distance of the center pit outlet of end and atomizer is 0-0.5mm; Described atomization 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.
2. pressurized capillary electrochromatographevaporative evaporative light scattering detector according to claim 1, is characterized in that: described capillary chromatographic column is open tubular column or packed column or integral post.
3. pressurized capillary electrochromatographevaporative evaporative light scattering detector according to claim 1, is characterized in that: described atomization kapillary is tapered or cylindrical, and material is quartz capillary.
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| CN103884814B (en) * | 2014-04-17 | 2015-10-14 | 厦门大学 | Ten thousand volts of high-voltage electric fields strengthen liquid chromatographic system |
| CN106680353B (en) * | 2017-03-21 | 2019-04-16 | 上海通微分析技术有限公司 | A kind of electric chromatogram apparatus |
| CN116183705A (en) * | 2017-03-30 | 2023-05-30 | 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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| 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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| 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 (3)
| Title |
|---|
| James N. Alexander，IV.Evaporative Light Scattering Detection for Microcolumn Liquid Chromatography.《Journal of Microcolumn Swparations》.1998,第10卷(第6期),第491-502页. * |
| 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》.2009,第27卷(第5期),609-620. * |
| 毛细管电色谱和加压毛细管电色谱的进展与应用;吴漪等;《色谱》;20090930;第27卷(第5期);609-620 * |
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