CN104931636A - Ultraviolet capillary column detector based on CCD - Google Patents
Ultraviolet capillary column detector based on CCD Download PDFInfo
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- CN104931636A CN104931636A CN201510350820.8A CN201510350820A CN104931636A CN 104931636 A CN104931636 A CN 104931636A CN 201510350820 A CN201510350820 A CN 201510350820A CN 104931636 A CN104931636 A CN 104931636A
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Abstract
An ultraviolet capillary column detector based on CCD comprises an ultraviolet capillary column chromatographic separation system, a CCD chromatography spectrum detector and a linkage control PC, wherein the ultraviolet capillary column chromatographic separation system is connected with the CCD chromatography spectrum detector, the linkage control PC is in control connection with the ultraviolet capillary column chromatographic separation system and the CCD chromatography spectrum detector, and the CCD chromatography spectrum detector comprises a nano-flow detecting pond, a detecting light source, a CCD spectrograph, a guide-in optical fiber and a receiving optical fiber. The ultraviolet capillary column detector has the advantages the detector is good in index consistency, high in sensitivity, low in power consumption, high in resolution, high in reading speed rate, low in cost and miniature, a new and efficient detecting manner is provided to the chromatography field, sample chromatography and spectrum information can be obtained at the same time in one operation, a large amount of time and cost of chromatographic analysis are saved, and the detector has advantages in the analysis of complex samples such as biology, medicine and food.
Description
Technical field
The present invention relates to multi-wavelength ultraviolet-visible detector, particularly relate to a kind of based on detector on the ultraviolet capillary column of CCD.
Background technology
Multi-wavelength ultraviolet-visible detector in liquid chromatography all has response to the material of ultravioletvisible absorption that has accounting for the material sum overwhelming majority, simultaneously under various conditions can steady operation and have very wide linear working range.Multi-wavelength ultraviolet-visible absorption detecting device can measure the chromatographic signal of multiple wavelength simultaneously, realizes identification chromatography peak and the purity determining peak.
Being applied to the modal multiwavelength detector of chromatogram at present is in the world diode array detector (Diode array detector, DAD are also PDA).DAD detecting device adopts the linear array of multiple photodiode, and by the restriction of technique and pixel dimension, the unit number of DAD is not high, and spectral resolution is relatively limited; And the workload of its data acquisition is on the other hand very large, require higher to electronic system.
Summary of the invention
Based on this, for above-mentioned technical matters, provide a kind of based on detector on the ultraviolet capillary column of CCD.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of based on detector on the ultraviolet capillary column of CCD, comprise chromatographic fractionation system on ultraviolet capillary column, CCD chromatogram spectroscopic detector and coordinated signals PC, on described ultraviolet capillary column, chromatographic fractionation system is connected with CCD chromatogram spectroscopic detector, chromatographic fractionation system and CCD chromatogram spectroscopic detector control linkage on described coordinated signals PC and described ultraviolet capillary column, described CCD chromatogram spectroscopic detector comprises receives upgrading detection cell, detection light source, CCD spectrometer, import optical fiber and receive optical fiber, described receive upgrading detection cell in there is rectangle cell cavity, and these four sides receiving upgrading detection cell have cross distribution and four passages be communicated with described cell cavity, described detection light source and CCD spectrometer are connected with described importing optical fiber and one end of receiving optical fiber respectively, the other end of described importing optical fiber and reception optical fiber stretches in described cell cavity through described passage respectively, on described outer capillary column, the capillary chromatographic column of chromatographic fractionation system to stretch in described cell cavity and with described importing optical fiber and receive optical fiber cross and cross, and the detection window of this capillary chromatographic column is positioned at the cross intersection of three, described CCD spectrometer is also connected with described coordinated signals PC.
Described upgrading detection cell of receiving comprises metab and upper buckle closure, the middle part of described metab has pond groove, described four passages are positioned at described metab, the entrance of this passage all has fixing described importing optical fiber, receives the Peek nut of optical fiber and capillary chromatographic column, the corner of described upper buckle closure is fixed by M4 hexagon socket cap head screw and described metab, and on this, buckle closure and described pond groove surround and form described cell cavity.
The middle part of described upper buckle closure has observation panel, is provided with M4 fluting flush end holding screw in this observation panel.
On described ultraviolet capillary column, chromatographic fractionation system comprises two high-pressure pumps, microfluidic mixer valve, automatic sampler, quantitative sample injection valve, four-way diverting valve, backpressure valve, capillary chromatographic column, damping fluid bottle, flow-limiting valve and high-voltage power supply, described two high-pressure pumps are communicated with described microfluidic mixer valve, described microfluidic mixer valve is connected with described quantitative sample injection valve through described automatic sampler, four ports of described four-way diverting valve connect described quantitative sample injection valve respectively, the positive pole of high-voltage power supply, the inlet end of backpressure valve and capillary chromatographic column, the endpiece of described capillary chromatographic column is connected with described flow-limiting valve, in described damping fluid bottle, there is damping fluid, described flow-limiting valve accesses in described damping fluid, the negative pole of described high-voltage power supply accesses in described damping fluid.
There is in the groove of described pond the rubber blanket covering described importing optical fiber and receive optical fiber.
Described detection light source is deuterium lamp.
Described detection window is quartz window.
The present invention is simple to operate, stable performance, indicator consilience is good, highly sensitive, and the present invention is based on CCD, there is low-power consumption, high resolving power, high read-out speed, low cost, and the feature of microminiaturization, for chromatographic field provides a kind of efficient detection means newly, on ultraviolet capillary column, the coupling of chromatographic fractionation system and CCD chromatogram spectroscopic detector contributes to the sensitivity improving CCD detecting device, and the information of sample chromatogram and spectrum can be obtained in single job simultaneously, save stratographic analysis a large amount of time and expense, for biology, medicine, analysis its advantage more aobvious of the complex samples such as food.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail:
Fig. 1 is modular structure schematic diagram of the present invention;
Fig. 2 is structural representation of the present invention;
Fig. 3 be of the present invention receive upgrading detection cell structural representation;
Fig. 4 is the spectrogram of the deuterium lamp of embodiment of the present invention experiment;
Fig. 5 is the naphthalene of embodiment of the present invention experiment, the separate colors spectrogram of anthracene;
Fig. 6 is the naphthalene of embodiment of the present invention experiment, the three-dimensional full-wave long scan figure of anthracene.
Embodiment
As shown in Figure 1, a kind of based on detector on the ultraviolet capillary column of CCD, comprise chromatographic fractionation system 1100 on ultraviolet capillary column, CCD chromatogram spectroscopic detector 1200 and coordinated signals PC1300, on ultraviolet capillary column, chromatographic fractionation system 1100 is connected with CCD chromatogram spectroscopic detector 1200, chromatographic fractionation system 1100 and CCD chromatogram spectroscopic detector 1200 control linkage on coordinated signals PC1300 and ultraviolet capillary column, realize chromatographic fractionation system 1100 on ultraviolet capillary column and control with the fully automation coupling of CCD chromatogram spectroscopic detector 1200.
CCD (charge-coupled device, charge coupled cell) be photosensitive detection device based on MOS technology, its maximum feature is using electric charge as signal, instead of common with voltage or electric current for signal, the whole course of work is the generation of electric charge, storage, transmission and detection.Ccd array detecting device (CCD array detector) to grow up a kind of optical multichannel detectors based on charge-coupled image sensor.Since first the beginning of the seventies is invented by BELL laboratory, CCD is just because high sensitivity, extremely wide spectral response range and dynamic range are subject to paying close attention to of people.With common photomultiplier (PMT), the optical detection devices such as photodiode array (PDA) and charge injection device (CID) are compared, it is wide that CCD has spectral response range, detection limit is low, quantum efficiency is high, wide dynamic range, and dark current is low with reading noise, manufacture volume is little, and low in energy consumption and hyperchannel such as to detect at the advantage simultaneously.At present, CCD has been widely used in the fields such as shooting, surveillance, astronomical sight, military affairs and spectral analysis.Optical imagery is carried out as famous Hubble just employs CCD technology.CCD is in the application in analysis field first from spectral analysis field, and based on the CCD-AES of CCD technology, the spectral detection researchs such as CCD-ICP-AES have extensively been carried out, and achieves multielement and detects simultaneously, also can obtain spectral background simultaneously.
On ultraviolet capillary column, chromatographic fractionation system 1100 contributes to the coupling of CCD chromatogram spectroscopic detector 1200 sensitivity improving CCD chromatogram spectroscopic detector 1200, and the information of sample chromatogram and spectrum can be obtained in single job simultaneously, save stratographic analysis a large amount of time and expense, for analysis its advantage more aobvious of the complex samples such as biology, medicine, food.
As shown in Figure 2, on ultraviolet capillary column, chromatographic fractionation system 1100 comprises two high-pressure pumps 1110, microfluidic mixer valve 1120, automatic sampler 1130, quantitative sample injection valve 1140, four-way diverting valve 1150, backpressure valve 1160, capillary chromatographic column 1170, damping fluid bottle 1180, flow-limiting valve 1190 and high-voltage power supply 1198.
Two high-pressure pump 1110 one end are communicated with two solvent bottles 1199 respectively, the other end is communicated with microfluidic mixer valve 1120, microfluidic mixer valve 1120 is connected with quantitative sample injection valve 1140 through automatic sampler 1130, four ports of four-way diverting valve 1150 connect quantitative sample injection valve 1140 respectively, the positive pole of high-voltage power supply 1198, the inlet end of backpressure valve 1160 and capillary chromatographic column 1170, the endpiece of capillary chromatographic column 1170 is connected with flow-limiting valve 1190, in damping fluid bottle 1180, there is damping fluid, flow-limiting valve 1190 accesses in damping fluid, in the negative pole access damping fluid of high-voltage power supply 1198.
Wherein, the mobile phase kind of damping fluid experimentally in system and determining.
High-pressure pump 1110 can ensure liquid in solvent bottle 1199 under hydraulic action by capillary chromatographic column 1170, Absorbable organic halogens conveying hundred receive upgrading flow, and it is adjustable to realize Gradient program, under High Pressure, can the generation of bubble in control separation system effectively.
Microfluidic mixer valve 1120 can realize the gradient mixing of binary solvent, while guarantee mixing efficiency, inhibits the time delay of gradient, ensure that accuracy and the reappearance of analysis.Before maintaining the constant post in separation capillary chromatographic column 10 front end, pressure is the key of stable system, solvent is pumped with the form of constant current by high-pressure pump 1110, the form transferring constant voltage at four-way diverting valve 1150 place to drives, and is coordinated realize pressure-driven internal solvent and sample enters capillary chromatographic column 1170 by four-way diverting valve 1150 and backpressure valve 1160.The effect of flow-limiting valve 1190 keeps certain pressure at the endpiece of capillary chromatographic column 1170, thus the formation of the bubble suppressing pressure abrupt change to cause, ensure the stability of system.
Automatic sampler 1130 can carry out two-forty sample introduction and multiclass analyzing and processing, it has carried out careful consideration to the material for the pin of sample introduction, valve and other streams, and syringe needle cleaning function is provided, cross pollution (residue) can be reduced to greatest extent, the sample drawn pushes quantitative sample injection valve 1140, and it adopts the mode of external quantitative loop in order to ensure accuracy and the precision of sample introduction.
High-voltage power supply 1198 adds electroosmotic flow on the basis of pressure current, realizes driving and quick separating the pressure of capillary chromatographic column 1170 internal solvent and sample and electric field simultaneously.Its positive pole is connected with four-way diverting valve 1150, and negative pole inserts in the damping fluid of damping fluid bottle 1180, is free to add generating positive and negative voltage at capillary chromatographic column 1170 two ends.
Particularly, CCD chromatogram spectroscopic detector 1200 comprise receive upgrading detection cell 1210, detection light source 1220, CCD spectrometer 1230, import optical fiber 1240 and receive optical fiber 1250.
Wherein, as shown in Figure 3, receive upgrading detection cell 1210 in there is rectangle cell cavity, and this receive upgrading detection cell four sides there is cross distribution and four passages be communicated with described cell cavity.
Detection light source 1220 and CCD spectrometer 1230 respectively with import optical fiber 1240 and one end of receiving optical fiber 1250 is connected, the other end importing optical fiber 1240 and reception optical fiber 1250 stretches in cell cavity through above-mentioned passage respectively, on outer capillary column, the capillary chromatographic column 1170 of chromatographic fractionation system 1100 to stretch in cell cavity and with importing optical fiber 1240 and receive optical fiber 1250 cross and cross, and the detection window of this capillary chromatographic column 1170 is positioned at the cross intersection of three.
The spectral response wave band of CCD spectrometer 1230 is 200nm-900nm, and pixel count is Unit 2048.Ccd signal adopts Serial output, and basic sweep frequency is 10 hardwoods/second (variable), and data bits is 16.Adopt flat field grating monochromator structure, realize when sample carries out time scan and length scanning detection through detection cell to the full absorbance measuring wave band incident light simultaneously.Along with the flowing of sample, the absorbance relative time of flowable component and the change of wavelength can be detected simultaneously, become the two-dimensional detector that simultaneously can detect chromatographic characterization and spectral characteristic.
Wherein, detection window is quartz window, ensures that transmission region is at 200nm-900nm, thus ensures that system realizes high-sensitivity measurement.
CCD spectrometer 1230 is also connected with coordinated signals PC1300, adjusts the gain of CCD spectrometer 1230, the relation between time shutter and output analog voltage, determine the sample frequency of CCD driving circuit thus ensure its measuring accuracy by coordinated signals PC1300.
Particularly, upgrading detection cell 1210 of receiving comprises metab 1211 and upper buckle closure 1212, the middle part of metab 1211 has pond groove 1213, above-mentioned four passages are positioned on metab 1211, the entrance of this passage all has the fixing Peek nut 1214 importing optical fiber 1240, receive optical fiber 1250 and capillary chromatographic column 1170, the corner of upper buckle closure 1212 is fixed by M4 hexagon socket cap head screw 1215 and metab 1211, and on this, buckle closure 1212 and pond groove 1213 surround and form above-mentioned cell cavity.
In order to observe the detection window of capillary chromatographic column 1170 and importing optical fiber 1240 and the position receiving optical fiber 1250 when assembling, to guarantee that three aligns, the middle part of upper buckle closure 1212 has observation panel 1212a, M4 fluting flush end holding screw 1212b is provided with in this observation panel 1212a, after determining that all parts all tighten up connection, tighten M4 fluting flush end holding screw 1212b, the interference of parasitic light can be avoided.
There is in pond groove 1213 rubber blanket 1216 covering and import optical fiber 1240 and receive optical fiber 1250, importing optical fiber 1240 and reception optical fiber 1250 are protected.
From detection light source 1220 light signal by import optical fiber 1240 enter receive upgrading detection cell 1210, in detection cell 1210, spectral signal weakens the absorption of characteristic wave bands due to sample, through light signal import CCD spectrometer 1230 by reception optical fiber 1250 again, the digital signal of generation imports coordinated signals PC1300 and carries out next step Data Management Analysis.
Wherein, detection light source 1220 is deuterium lamp, and its radiation wave band is 180nm-400nm, and integrated shutter can realize quick, the stable output of spectrum.The requirement of detection system to baseline and drift to be met in temperature stability, time stability, adopt constant current constant voltage twice control method to stablize output, make light source stability be less than 0.05%/h.Certainly, also can be other light sources.
The course of work of the present invention is as follows:
Mobile phase solvent pumps into microfluidic mixer valve 1120 by solvent bottle 1199 through high-pressure pump 1110, the gradient mixing of binary solvent can be realized, the sample that automatic sampler 1130 is drawn pushes quantitative sample injection valve 1140, solvent and sample are pumped with the form of constant current by high-pressure pump 1110, the form transferring constant voltage at four-way diverting valve 1150 place to drives, coordinated by four-way diverting valve 1150 and backpressure valve 1160 and realize pressure-driven internal solvent and sample enters capillary chromatographic column 1170, the effect of flow-limiting valve 1190 keeps certain pressure at the endpiece of capillary chromatographic column 1170, thus the formation of the bubble suppressing pressure abrupt change to cause, the stability of guarantee system, high-voltage power supply 1198 adds electroosmotic flow on the basis of pressure current, one termination electrode is connected with four-way diverting valve 1150, one termination electrode inserts in damping fluid bottle 1180, realize driving and quick separating the pressure of separation capillary chromatographic column 10 internal solvent and sample and electric field simultaneously, deuterium lamp by import optical fiber 1240 enter receive upgrading detection cell 1210 be irradiated on the sample of separation, because sample weakens the absorption of characteristic wave bands, through light signal again by reception optical fiber 1250 import CCD spectrometer 1230, the digital signal produced imports coordinated signals PC1300 and carries out next step Data Management Analysis, and the fully automation realizing chromatographic fractionation system 1100 and CCD chromatogram spectroscopic detector 1200 on ultraviolet capillary column controls, obtain miniature miniflow CCD UV detect chromatogram spectrogram.
To detect palycyclic aromatic:
Experiment condition
Test sample: naphthalene, anthracene;
Sample concentration: 1 × 10-5g/ml;
Capillary chromatographic column model: EP-100-20/45-3-C18;
Mobile phase: acetonitrile: water=70:30;
Flow rate of mobile phase: 0.08ml/min (split ratio 100:1);
High-voltage power supply :-15KV;
Column flow rate: 800nL/min;
Pump pressure: 15.4MPa;
Sample size: 15nL;
Determined wavelength: 220nm, 251nm dual-wavelength simultaneous detection.
Fig. 4 is the spectrogram of deuterium lamp, can find out, the wavelength coverage of the light sent is generally the continuous light bands of a spectrum of 190-400nm, has characteristic spectral line at 486.0nm, 583.0nm place, and strong, the stable spectrum that can produce 215-300nm exports.
Fig. 5 is the separate colors spectrogram of naphthalene, anthracene, and can find out that both achieve good separation in 6min, and sample peak shape is fine, peak is without hangover and phenomenon of protracting, and symmetry is good.The peak at 3.34min place is naphthalene, peak height 61.16mAu (220nm), and the peak at peak area accounting 44.5%, 5.24min place is anthracene, peak height 100.05mAu (changing 251nm into), peak area accounting 48.6%.This experiment adopts multi-wavelength to monitor simultaneously, can detect, improve the sensitivity of detection and reduce detectability at the optimal wavelength of naphthalene and anthracene.
Fig. 6 is the three-dimensional full-wave long scan figure of naphthalene, anthracene, abscissa axis (X-axis) is chromatographic retention, axis of ordinates (Y-axis) is spectrum all-wave long (this experiment is set as 200-300nm), and Z axis is for absorbing light intensity (mAu).In three-dimensional plot, two sample peaks at 3.34min place and 5.24min place can be seen equally, and can find out that the maximum absorption wavelength of naphthalene is 220nm, and the maximum absorption wavelength of anthracene is 251nm.By the long spectrogram of three-dimensional full-wave, two-dimensional detection and analysis are carried out to interested wavelength segment.
But, those of ordinary skill in the art will be appreciated that, above embodiment is only used to the present invention is described, and be not used as limitation of the invention, as long as in spirit of the present invention, all will drop in Claims scope of the present invention the change of the above embodiment, modification.
Claims (7)
1. one kind based on detector on the ultraviolet capillary column of CCD, it is characterized in that, comprise chromatographic fractionation system on ultraviolet capillary column, CCD chromatogram spectroscopic detector and coordinated signals PC, on described ultraviolet capillary column, chromatographic fractionation system is connected with CCD chromatogram spectroscopic detector, chromatographic fractionation system and CCD chromatogram spectroscopic detector control linkage on described coordinated signals PC and described ultraviolet capillary column, described CCD chromatogram spectroscopic detector comprises receives upgrading detection cell, detection light source, CCD spectrometer, import optical fiber and receive optical fiber, described receive upgrading detection cell in there is rectangle cell cavity, and these four sides receiving upgrading detection cell have cross distribution and four passages be communicated with described cell cavity, described detection light source and CCD spectrometer are connected with described importing optical fiber and one end of receiving optical fiber respectively, the other end of described importing optical fiber and reception optical fiber stretches in described cell cavity through described passage respectively, on described outer capillary column, the capillary chromatographic column of chromatographic fractionation system to stretch in described cell cavity and with described importing optical fiber and receive optical fiber cross and cross, and the detection window of this capillary chromatographic column is positioned at the cross intersection of three, described CCD spectrometer is also connected with described coordinated signals PC.
2. according to claim 1 a kind of based on detector on the ultraviolet capillary column of CCD, it is characterized in that, described upgrading detection cell of receiving comprises metab and upper buckle closure, the middle part of described metab has pond groove, described four passages are positioned at described metab, the entrance of this passage all has fixing described importing optical fiber, receives the Peek nut of optical fiber and capillary chromatographic column, the corner of described upper buckle closure is fixed by M4 hexagon socket cap head screw and described metab, and on this, buckle closure and described pond groove surround and form described cell cavity.
3. according to claim 2ly a kind ofly to it is characterized in that based on detector on the ultraviolet capillary column of CCD, the middle part of described upper buckle closure has observation panel, is provided with M4 and slots flush end holding screw in this observation panel.
4. a kind of based on detector on the ultraviolet capillary column of CCD according to claim 1 or 3, it is characterized in that, on described ultraviolet capillary column, chromatographic fractionation system comprises two high-pressure pumps, microfluidic mixer valve, automatic sampler, quantitative sample injection valve, four-way diverting valve, backpressure valve, capillary chromatographic column, damping fluid bottle, flow-limiting valve and high-voltage power supply, described two high-pressure pumps are communicated with described microfluidic mixer valve, described microfluidic mixer valve is connected with described quantitative sample injection valve through described automatic sampler, four ports of described four-way diverting valve connect described quantitative sample injection valve respectively, the positive pole of high-voltage power supply, the inlet end of backpressure valve and capillary chromatographic column, the endpiece of described capillary chromatographic column is connected with described flow-limiting valve, in described damping fluid bottle, there is damping fluid, described flow-limiting valve accesses in described damping fluid, the negative pole of described high-voltage power supply accesses in described damping fluid.
5. according to claim 4ly a kind ofly to it is characterized in that based on detector on the ultraviolet capillary column of CCD that there is in the groove of described pond the rubber blanket covering described importing optical fiber and receive optical fiber.
6. according to claim 5ly a kind ofly to it is characterized in that based on detector on the ultraviolet capillary column of CCD, described detection light source is deuterium lamp.
7. according to claim 6ly a kind ofly to it is characterized in that based on detector on the ultraviolet capillary column of CCD, described detection window is quartz window.
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| CN201510350820.8A CN104931636B (en) | 2015-06-23 | 2015-06-23 | Based on detector on the ultraviolet capillary column of CCD |
| PCT/CN2016/070112 WO2016206355A1 (en) | 2015-06-23 | 2016-01-05 | Ultraviolet capillary column detector based on ccd |
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| CN201510350820.8A CN104931636B (en) | 2015-06-23 | 2015-06-23 | Based on detector on the ultraviolet capillary column of CCD |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016206355A1 (en) * | 2015-06-23 | 2016-12-29 | 阎超 | Ultraviolet capillary column detector based on ccd |
| CN107621387A (en) * | 2017-09-12 | 2018-01-23 | 河南科技大学第附属医院 | A kind of medical test sampler |
| CN113341021A (en) * | 2021-06-28 | 2021-09-03 | 南京无书化工有限公司 | Online monitoring method and system for oil gas of chromatographic-spectral combined transformer |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114460196B (en) * | 2022-01-28 | 2023-09-29 | 合肥高尔生命健康科学研究院有限公司 | Chromatographic analysis system for active ingredients in pesticide preparation |
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| US6428488B1 (en) * | 1997-08-28 | 2002-08-06 | Kenneth Kensey | Dual riser/dual capillary viscometer for newtonian and non-newtonian fluids |
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| WO2016206355A1 (en) * | 2015-06-23 | 2016-12-29 | 阎超 | Ultraviolet capillary column detector based on ccd |
| CN107621387A (en) * | 2017-09-12 | 2018-01-23 | 河南科技大学第附属医院 | A kind of medical test sampler |
| CN113341021A (en) * | 2021-06-28 | 2021-09-03 | 南京无书化工有限公司 | Online monitoring method and system for oil gas of chromatographic-spectral combined transformer |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104931636B (en) | 2016-06-22 |
| WO2016206355A1 (en) | 2016-12-29 |
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