CN2852130Y - Multifunctional high-performance liquid chromatography post column derivation analyzer - Google Patents
Multifunctional high-performance liquid chromatography post column derivation analyzer Download PDFInfo
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- CN2852130Y CN2852130Y CN 200520028456 CN200520028456U CN2852130Y CN 2852130 Y CN2852130 Y CN 2852130Y CN 200520028456 CN200520028456 CN 200520028456 CN 200520028456 U CN200520028456 U CN 200520028456U CN 2852130 Y CN2852130 Y CN 2852130Y
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Abstract
The utility model provides a multifunctional high-performance liquid chromatography post column derivation analyzer. A sampling device is composed of an HPLC pump, a sample injection device, a chromatographic column and a precise thermo tank. A derivation liquid injection device is composed of a plunger pump 1, a filter 2 and a one-way valve 2. The derivation liquid injection device is connected with the sampling device through a T-joint 1. A derivation liquid reaction device is composed of a mixer 1, a derivation reaction chamber, a one-way valve 3 and a diphase transfer valve 2. A neutralizer device is composed of a plunger pump 2, a filter 3, a one-way valve 5 and a break valve 1, and is connected with a T-joint 2 and the derivation liquid reaction device. A thermostatic apparatus is composed of a mixer 2, a constant temperature both, a one-way valve 4, a T-joint 3 and a filter 4, and is connected with the input terminal of the detector in the end and the output terminal of detector is connected to the waste fluid pool. After the separate matter of the high-efficient liquid-phase chromatographic column generates derivation reaction through acid or alkali derivation solution, the ultraviolet (VWD) detector discrimination is realized, and the utility model is suitable to the DAD digit detector, and the visible -ultraviolet light (UV-Vis) detector or fluorescence detector.
Description
Technical field
The utility model provides deriveding analysis instrument behind a kind of multifunctional efficient liquid-phase chromatographic column, belongs to the analytical chemistry instrument equipment technical field.
Background technology
Deriving technology is high performance liquid chromatography (High PerformanceLiquid Chromatography, HPLC) development of isolation technics behind the performance liquid chromatographic column.The detecting device that the high performance liquid chromatography authentication technique is adopted generally is a UV-detector, but has a lot of materials not absorb at the ultraviolet spectrum wave band, and perhaps the absorption energy of ultraviolet light is very low, has limited the application of UV-detector.
The post-column derivation technology is with the isolated material of performance liquid chromatographic column, carry out chemical reaction by a kind of special device again and make it to derive for material or generate fluorophor, realize that visible/ultraviolet light (UV/Vis) detecting device or fluorescence detector differentiate with visible/ultraviolet light (UV/Vis) absorption effect.
Existing a kind of post-column derivation technology is that the solution that isolated material of performance liquid chromatographic column and constant flow pump are imported is converged, and after adding thermal response, differentiates through fluorescence detector again.Though, the discriminating that this device can be realized some compound for example: amino acid, fluorescence detector has significant limitation, chemical compound lot can not be realized differentiating, and detection sensitivity is very low.
UV-detector (VWD) is a detecting device the most frequently used in the HPLC system, and in the direct chromatogram of all micro substances was differentiated, UV-detector (VWD) detection sensitivity was the highest; But the erosion that UV-detector (VWD) can not be born acid or alkaline solution can not change the interference that can not bear pulse solution by bearing temperature.
Summary of the invention
The utility model provides deriveding analysis instrument behind a kind of multifunctional efficient liquid-phase chromatographic column, the material that its purpose is separated performance liquid chromatographic column is after peracid or alkali derivative solution derivatization reaction, realize the discriminating of ultraviolet (VWD) detecting device, and be applicable to DAD digital detector, visible-ultraviolet light (UV-Vis) detecting device or fluorescence detector.
Technical solution of the present utility model is as follows:
Connect and compose sampling device by pipeline in order by HPLC pump, pressure transducer, filtrator, injector, chromatographic column, exact constant temperature case, pressure transducer, retaining valve, two-phase transfer valve, connect and compose the liquid injection device of deriving by pipeline in order by ram pump, pressure transducer, filtrator, retaining valve, be connected with sampling device by threeway, mixer and derivatization reaction case, retaining valve, two-phase transfer valve connect and compose the liquid reaction unit of deriving by pipeline in order; Connect and compose the neutralizer device by pipeline in order by ram pump, pressure transducer, filtrator, retaining valve, stop valve, be connected with threeway, the liquid reaction unit of deriving, mixer, calibration cell, retaining valve, threeway, filtrator connect and compose thermostat by pipeline in order, connect the detecting device input end at last, the output terminal of detecting device is connected to waste liquid pool.Wherein, the HPLC pump is connected with the moving phase pond; Ram pump is connected with the liquid pool of deriving; Ram pump with in be connected with liquid pool; Ram pump with in be connected with liquid pool; The termination waste liquid pool in addition of two-phase transfer valve, the two-phase transfer valve connects threeway, and stop valve is connected between waste liquid pool and the retaining valve.
Described detecting device can be UV-detector (VWD) or DAD digital detector, visible-ultraviolet light (UV-Vis) detecting device or fluorescence detector.
The middle part of above-mentioned derivatization reaction case is a well heater, and uniform winding has the reaction tube that resistant material is made on it, also can be provided with heating arrangement outside corrosion resistant reaction tank, and well heater is connected with Constant temp. regulating device by digital temperature sensor;
Calibration cell connects and composes thermostat by semiconductor thermostat, reaction tube or reaction tank.
The column device that mixer is filled by the anisodiametric Ceramic Balls of diameter phi 0.1mm～φ 1mm.
Described pressure transducer, retaining valve, two-phase transfer valve, stop valve are connected in the native system as the system protection parts.
Pressure transducer: ceramic condenser pressure unit
Injector: HPLC system-specific injector
Chromatographic column: HPLC system-specific analytical column
Filtrator: aperture φ 0.4 μ m polytetrafluoroethylmaterial material filter membrane
Retaining valve: resistant material is made
Method is switched in two-phase: resistant material is made
Stop valve: resistant material is made
Threeway: resistant material is made and is not had a dead point
HPLC pump: HPLC system-specific infusion pump
Ram pump: resistant material is made twin columns stopper rod pump
Moving phase pond, waste liquid pool, the liquid pool of deriving, in and liquid pool be general vial
Exact constant temperature case: the precise constant-temperature equipment that adopts digital temperature sensor, PID to regulate
Detecting device: UV-detector (VWD), DAD digital detector, visible-ultraviolet light (UV-Vis) detecting device or fluorescence detector
The course of work of the present utility model is as follows:
Sample to be analyzed injects through injector according to the HPLC analysis condition;
According to the HPLC analysis condition, HPLC pump 1 input moving phase is injected chromatographic column 5 through pressure transducer 2, filtrator 4 by injector 3, filtrator 4;
Sample separates after pressure transducer 7 retaining valves 8, two-phase transfer valve 9 converge in threeway 14 and derivatization reaction liquid through chromatographic column 5, enter derivatization reaction case 21 through mixer 20 and carry out chemical reaction, derivatization reaction liquid converges in threeway 24 through retaining valve 22, two-phase transfer valve 23 and neutralization reaction liquid and enters detecting device 30 through mixer 25, calibration cell 26, retaining valve 27, threeway 28, filtrator 29 and enter waste liquid pool again;
Use UV-Vis detecting device 30 or fluorescence detector to detect, close stop valve 19, sample meets at threeway 14, enters waste liquid pool through mixer 20, derivatization reaction case 21, retaining valve 22, threeway 24, mixer 25, calibration cell 26, retaining valve 27, threeway 28, filtrator 29 after entering detecting device 30 through retaining valve 8, two-phase transfer valve 9 and derivatization reaction liquid through chromatographic column 5 separation;
Close stop valve 19, sample separates through chromatographic column 5 that to enter waste liquid pool again be classical H PLC analytic system after retaining valve 8, two-phase transfer valve 9, threeway 14, mixer 20, derivatization reaction case 21, retaining valve 22, two-phase transfer valve 23, threeway 24, filtrator 29 enter detecting device 30;
The liquid of deriving is joined at threeway 14 and chromatographic column separator through ram pump 10, pressure transducer 11, filtrator 12, retaining valve 13;
Neutralizer converges at threeway 24 and post-column derivation liquid branch through ram pump 15, pressure transducer 16, filtrator 17, retaining valve 18, stop valve 19;
After testing finished, cleaning fluid injected chromatographic column 5 through retaining valve 8, two-phase transfer valve 9 through the HPLC infusion pump, and washing lotion enters waste liquid pool;
After testing finishes, the liquid pool splendid attire cleaning fluid of deriving, inject filtrator 12, retaining valve 13, threeway 14, mixer 20, derivatization reaction case 21, retaining valve 22, two-phase transfer valve 23, threeway 24 and process filter 29, detecting device 30 through ram pump 10, washing lotion enters waste liquid pool;
After testing finishes, close stop valve 31, in and liquid pool splendid attire cleaning fluid inject through ram pump 15, filter rinsed 17, retaining valve 18, stop valve 19, threeway 24, mixer 25, calibration cell 26, single-phase valve 27, threeway 28, filtrator 29, detecting device 30, washing lotion enters waste liquid pool;
Close stop valve 19, in and liquid pool splendid attire cleaning fluid inject through ram pump 15, filter rinsed 17, retaining valve 18, stop valve 31, washing lotion enters waste liquid pool;
Advantage of the present utility model is: the material that performance liquid chromatographic column separates can access neutralisation treatment after peracid or alkali are derived the liquid reaction, the pH value of its liquid of deriving is reached in pH4～pH8 scope, is more suitable for UV-detector (VWD) discriminating.
Of the present utility modelly be also advantageous in that material that performance liquid chromatographic column separates and acid or alkalescence are derived and obtain mixing after liquid converges and handle, make the material of its chromatographic column separation can participate in chemical reaction fully; And this mixer has also played buffer action, has reduced the acid of ram pump input or the flow pulses of alkaline derivative solution, has reduced the flow pulses of the neutralization solution of ram pump input, and it is more steady that derivatization reaction liquid enters UV-detector.
The derivatization reaction liquid that is also advantageous in that of the present utility model can carry out the temperature control and treatment, make its chemical reaction of deriving thorough, and the liquid of deriving enters detecting device with its suitable temperature, avoided too high or low excessively the influence of temperature, eliminated the interference of temperature variation detection sensitivity to the detecting device detection cell.
Many retaining valves, the stop valve control measure that are also advantageous in that the chemical reaction system of deriving is taked of the present utility model are avoided artificial or other factors cause acid or the recoil of alkaline derivative solution to the destruction of chromatographic column and the interference of derivatization reaction.
Of the present utility model being also advantageous in that adopted untouchable pressure transducer, automatically to HPLC infusion pump, the fluid column plug infusion pump of deriving, neutralizer plunger infusion pump pressure control in the system, guarantees gentle, the flow speed stability of derivatization reaction.
Of the present utility model being also advantageous in that adopted corrosion resistant pot strainer in the system, avoid large granular impurity block system and detecting device.
Of the present utility model being also advantageous in that can realize easily that after testing finishes chromatographic column, pipeline and detecting device etc. independently clean separately.
Detection liquid and the cleaning fluid of being also advantageous in that of the present utility model can both realize concentrating recovery, and composing environment pollutes.
Description of drawings
Fig. 1 is the utility model structure principle chart.
Embodiment
According to shown in Figure 1, connect and compose sampling device by pipeline in order by HPLC pump 1, pressure transducer 2, filtrator 4, injector 3, chromatographic column 5, exact constant temperature case 6 and pressure transducer 7, retaining valve 8, two-phase transfer valve 9, connect and compose the liquid injection device of deriving by pipeline in order by ram pump 10, pressure transducer 11, filtrator 12, retaining valve 13, be connected with sampling device by threeway 14, mixer 20 and derivatization reaction case 21, retaining valve 22, two-phase transfer valve 23 connect and compose the liquid reaction unit of deriving by pipeline in order; Connect and compose the neutralizer device by pipeline in order by ram pump 15, pressure transducer 16, filtrator 17, retaining valve 18, stop valve 19, be connected with threeway 24, the liquid reaction unit of deriving, mixer 25, calibration cell 26, retaining valve 27, threeway 28, filtrator 29 connect and compose thermostat by pipeline in order, connect detecting device 30 input ends at last, the output terminal of detecting device 30 is connected to waste liquid pool; Wherein, HPLC pump 1 is connected with the moving phase pond; Ram pump 10 is connected with the liquid pool of deriving; Ram pump 15 with in be connected with liquid pool; The termination waste liquid pool in addition of two-phase transfer valve 9, two-phase transfer valve 23 connects threeway 28; Stop valve 31 is connected between waste liquid pool and the retaining valve 18;
Following examples further specify the utility model
(1) quality discrimination of Alprostadil:
Precision takes by weighing Alprostadil 10mg, moving phase solution preparation with acetonitrile-phosphate buffer (pH6.3) (3: 2) contains Alprostadil 20 μ g/ml solution, gets 20 μ l and injects injector, the mobile liquid that mixes of HPLC infusion pump input, flow velocity 1ml/min, the Alprostadil sample separates through chromatographic column; Preparation 1M potassium hydroxide solution, potassium hydroxide solution injects through ram pump 1, and flow velocity 1.5ml/min regulates derivatization reaction oven temperature, degree and thermostatic control at 45 ℃; Preparation 0.2N hydrochloric acid solution injects dilute hydrochloric acid solution through ram pump 2, flow velocity 0.5ml/min regulates calibration cell temperature and thermostatic control at 25 ℃; Set UV-detector (VWD) and detect wavelength 278nm, the record chromatographic curve.
(2) prostaglandin A
1Quality discrimination:
Precision takes by weighing prostaglandin A
15mg is with the moving phase solution preparation prostaglandin-containing A of acetonitrile-phosphate buffer (pH6.3) (3: 2)
12 μ g/ml solution are got 50 μ l and are injected injector, the mobile liquid that mixes of HPLC infusion pump input, flow velocity 1ml/min, prostaglandin A
1Sample separates through chromatographic column; Preparation 1M potassium hydroxide solution injects potassium hydroxide solution through ram pump 1, flow velocity 0.85ml/min regulates derivatization reaction oven temperature, degree and thermostatic control at 60 ℃; Preparation 0.2N hydrochloric acid solution injects dilute hydrochloric acid solution through ram pump 2, flow velocity 0.5ml/min regulates calibration cell temperature and thermostatic control at 25 ℃; Set UV-detector (VWD) and detect wavelength 278nm, the record chromatographic curve.
(3) mensuration of the remaining lactone of POTASSIUM DEHYDRO-OGRAPHOLIDE SUCCINATE
Precision takes by weighing andrographolide succinic acid half-ester monopotassium salt 10mg, moving phase solution preparation with methanol-water (3: 2) contains andrographolide succinic acid half-ester monopotassium salt 200 μ g/ml solution, get 50 μ l and inject injector, the mobile liquid that mixes of HPLC infusion pump input, flow velocity 1ml/min, andrographolide succinic acid half-ester monopotassium salt sample separates through chromatographic column; Preparation 1M sodium bicarbonate solution injects sodium bicarbonate solution through ram pump 1, flow velocity 1ml/min regulates derivatization reaction oven temperature, degree and thermostatic control at 65 ℃; Preparation 0.2N hydrochloric acid solution injects dilute hydrochloric acid solution through ram pump 2, flow velocity 1ml/min regulates calibration cell temperature and thermostatic control at 25 ℃; Set UV-detector (VWD) and detect wavelength 254nm, the record chromatographic curve.
(4) amino acid is differentiated
Chromatographic column: unmodified packed column
Moving phase: methanol-water (3: 2)
Derivatization reaction reagent: 1M sodium hydroxide solution or o-phthalaldehyde(OPA) (OPA) solution
Detecting device: fluorescence detector, excitation wavelength lambda
Ex330nm, emission wavelength lambda
Em465nm
The amino acid sample is injected by injector, HPLC infusion pump input moving phase, and flow velocity 1ml/min, the chromatographic column thermostatic control is at 40 ℃; Derivatization reaction liquid injects through ram pump 1, and flow velocity 0.5ml/min regulates derivatization reaction oven temperature, degree and thermostatic control at 100 ℃; Close stop valve 1, the liquid of deriving enters calibration cell through two-phase transfer valve 2, regulates calibration cell temperature and thermostatic control at 25 ℃; Set the fluorescence detector excitation wavelength lambda
Ex330nm; Emission wavelength lambda
Em465nm, the record chromatographic curve.
Claims (2)
1, deriveding analysis instrument behind a kind of multifunctional efficient liquid-phase chromatographic column, it is characterized in that: by HPLC pump (1), pressure transducer (2), filtrator (4), injector (3), chromatographic column (5), exact constant temperature case (6) and pressure transducer (7), retaining valve (8), two-phase transfer valve (9) connects and composes sampling device by pipeline in order, by ram pump (10), pressure transducer (11), filtrator (12), retaining valve (13) connects and composes the liquid injection device of deriving by pipeline in order, be connected mixer (20) and derivatization reaction case (21) with sampling device by threeway (14), retaining valve (22), two-phase transfer valve (23) connects and composes the liquid reaction unit of deriving by pipeline in order; Connect and compose the neutralizer device by pipeline in order by ram pump (15), pressure transducer (16), filtrator (17), retaining valve (18), stop valve (19), be connected with threeway (24), the liquid reaction unit of deriving, mixer (25), calibration cell (26), retaining valve (27), threeway (28), filtrator (29) connect and compose thermostat by pipeline in order, connect detecting device (30) input end at last, the output terminal of detecting device (30) is connected to waste liquid pool; Wherein, HPLC pump (1) is connected with the moving phase pond; Ram pump (10) is connected with the liquid pool of deriving; Ram pump (15) with in be connected with liquid pool; The termination waste liquid pool in addition of two-phase transfer valve (9), two-phase transfer valve (23) connects threeway (28); Stop valve (31) is connected between waste liquid pool and the retaining valve (18);
Described detecting device (30) is selected from UV-detector or DAD digital detector, visible-UV-detector or fluorescence detector.
2, analyser according to claim 1, it is characterized in that: the middle part of derivatization reaction case is a well heater, uniform winding has the reaction tube that resistant material is made on it, or outside corrosion resistant reaction tank, being provided with heating arrangement, well heater is connected with Constant temp. regulating device by digital temperature sensor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520028456 CN2852130Y (en) | 2005-04-01 | 2005-04-01 | Multifunctional high-performance liquid chromatography post column derivation analyzer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200520028456 CN2852130Y (en) | 2005-04-01 | 2005-04-01 | Multifunctional high-performance liquid chromatography post column derivation analyzer |
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| CN2852130Y true CN2852130Y (en) | 2006-12-27 |
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| CN 200520028456 Expired - Fee Related CN2852130Y (en) | 2005-04-01 | 2005-04-01 | Multifunctional high-performance liquid chromatography post column derivation analyzer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323361A (en) * | 2011-09-02 | 2012-01-18 | 浙江大学 | Post-column electrochemical derivatization apparatus for liquid chromatography |
| CN103808830A (en) * | 2014-03-10 | 2014-05-21 | 广东海洋大学 | Post-column derivatization type high-performance liquid chromatography |
| CN105044251A (en) * | 2015-07-28 | 2015-11-11 | 李绍平 | On-line micro-reaction device |
| CN107870219A (en) * | 2016-09-26 | 2018-04-03 | 中国科学院大连化学物理研究所 | A kind of small chemical derivatization device |
-
2005
- 2005-04-01 CN CN 200520028456 patent/CN2852130Y/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323361A (en) * | 2011-09-02 | 2012-01-18 | 浙江大学 | Post-column electrochemical derivatization apparatus for liquid chromatography |
| CN103808830A (en) * | 2014-03-10 | 2014-05-21 | 广东海洋大学 | Post-column derivatization type high-performance liquid chromatography |
| CN105044251A (en) * | 2015-07-28 | 2015-11-11 | 李绍平 | On-line micro-reaction device |
| CN107870219A (en) * | 2016-09-26 | 2018-04-03 | 中国科学院大连化学物理研究所 | A kind of small chemical derivatization device |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20061227 |