CN105486774A - Liquid chromatogram precolumn derivatization device - Google Patents
Liquid chromatogram precolumn derivatization device Download PDFInfo
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- CN105486774A CN105486774A CN201511031807.2A CN201511031807A CN105486774A CN 105486774 A CN105486774 A CN 105486774A CN 201511031807 A CN201511031807 A CN 201511031807A CN 105486774 A CN105486774 A CN 105486774A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
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Abstract
The invention discloses a liquid chromatogram precolumn derivatization device. The device comprises a liquid phase solution, a pump, a reaction device, a sample injector, an incubator chromatographic column and a detector which are sequentially connected, the reaction device comprises a shell, a reaction chamber and a temperature control unit, the reaction chamber is formed in the shell, one end of the reaction chamber is communicated with the pump, the other end of the reaction chamber is communicated with the sample injector, a heat-insulation layer is arranged on the outer wall of the reaction chamber, the temperature control unit comprises a temperature control panel ad a temperature control circuit board, a groove used for containing the temperature control panel is formed in the bottom end face of the reaction chamber, the temperature control panel is fixed into the groove and conducts temperature control on the reaction chamber, the device further comprises a spiral flow deflector, and the spiral flow deflector is arranged inside the reaction chamber and used for sufficiently mixing reaction liquid. The liquid chromatogram precolumn derivatization device is great in temperature and reaction time controllability and high in derivatization efficiency.
Description
Technical field
The present invention relates to chemical derivatization technical field, particularly relate to a kind of column front derivation device of liquid chromatography.
Background technology
Derivatization is that a kind of chemical transformation that utilizes becomes the material of similar chemical constitution converting compounds.In general, the compound of a specific function participates in derivatization reaction, and solubleness, boiling point, fusing point, aggregative state or chemical composition can produce and depart from.Consequent new chemical property can be used for quantizing or being separated.The effect of the derivatization of sample is mainly similar to its chemical constitution the Substance Transformation being difficult to analyze but is easy to the material analyzed, is convenient to quantification and is separated.When detection material is not easy detected, as without uv absorption etc., can processing, as added chromophore etc., generating the material that can be detected.Be widely used in instrumental analysis.In gas chromatography, applied chemistry derivatization reaction is volatile grade in order to increase sample or improves detection sensitivity, and the chemical derivatization of high performance liquid chromatography refers to and utilizes certain reagent (being generally called chemically derived reagent or labelled reagent) and sample component to carry out chemical reaction under certain condition, the product of reaction is conducive to chromatogram and detects or be separated.General chemical derivatization mainly contains following object: the sensitivity improving sample detection; Improve the degree of separation of sample mixture; Be suitable for doing Structural Identification further, as mass spectrum, infrared or nuclear magnetic resonance etc.Carry out chemically derived reaction and should meet following requirement: require not harsh to reaction conditions, and can carry out rapidly, quantitatively; Only generate a kind of derivant to certain component in sample, byproduct of reaction and excessive derivative reagent do not disturb the separation and detection of test sample product; Chemically derived reagent is conveniently easy to get, and versatility is good.
During liquid phase detects, in order to improve the detectability of determinand, the detection of some object needs, by first for determinand derivatization, then to make reactant on analytical column, realize separation and detect, the content of indirect reaction thing to be detected.Wherein, column front derivation and post-column derivation two kinds, pre-column derivatization and post-column derivation method respectively have its relative merits.The advantage of pre-column derivatization is: relatively freely select reaction conditions; There is not the restriction of reaction kinetics; The accessory substance of derivatization can carry out pre-service to reduce or to eliminate its interference; The carrying out of easy permission multistep reaction; More derivatization reagent is had to select; Do not need complicated instrument and equipment.Shortcoming is: the accessory substance of formation may cause larger difficulty to chromatographic resolution; In derivatization process, easily introduce impurity or Interference Peaks, or make sample loss.The advantage of post-column derivation method has: form accessory substance inessential, product does not need high stability yet, the repeatability only needed; Analyte can be separated under its original form, easily selects existing analytical approach.Shortcoming is: need extra equipment, higher to instrument requirements; Reactor can cause peak stretching, reduces resolution; Excessive reagent is had to cause interference.
Summary of the invention
The object of this invention is to provide a kind of can accurately to the column front derivation device of the liquid chromatography that reaction time, temperature of reaction control.
To achieve these goals, technical scheme provided by the invention is: the column front derivation device providing a kind of liquid chromatography, comprise: the liquid solution connected successively, pump, reaction unit, injector, insulation can chromatographic column, detecting device, described reaction unit comprises housing, reaction chamber and control temperature unit, described reaction chamber is located in described housing and one end and is communicated with described pump, the other end is communicated with described injector, and described reacting outdoor wall is provided with heat-insulation layer, described control temperature unit comprises temperature control panel and temperature-adjusting circuit plate, and described reaction chamber bottom face is provided with one for holding the groove of described temperature control panel, described temperature control panel to be fixed in described groove and to carry out temperature control to described reaction chamber, also comprise spiral deflector, it is inner that described spiral deflector is located at described reaction chamber.
Bottom described reaction chamber and top is respectively equipped with entrance and the outlet of liquid, and described entrance is communicated with described pump, and described outlet is communicated with described injector.
Described temperature control panel comprises rectangular-shaped main body sheet material, and described main body sheet material is fixed with some semiconductor chilling plates, and by some described semiconductor chilling plates and described reaction chamber lower surface close contact, and the part of described reaction chamber lower surface and described semiconductor chilling plate close contact is the sheet metal that heat conductivility is good.
In some described semiconductor chilling plates, be divided into two groups, first group is the one side and described reaction chamber lower surface close contact that heat, and second group is the one side and described reaction chamber lower surface close contact of freezing, and first group of semiconductor chilling plate and second group of spaced laying of semiconductor chilling plate.
Also temperature sensing device is provided with in described reaction chamber.
Also comprise control module, described temperature-adjusting circuit plate and described temperature sensing device are all connected with described control module, the temperature information that described control module is fed back by described temperature sensing device, and then control the work of described temperature-adjusting circuit plate.
Described housing is also provided with air inlet and air outlet, and described air inlet is located at described housing upper surface, and described air outlet is located at described housing lower surface, and described air outlet place is also provided with exhaust blower.
Also be provided with various way solenoid valve between described liquid solution and described pump, and described various way solenoid valve and described control module are electrically connected.
Compared with prior art, in the column front derivation device of liquid chromatography of the present invention, comprise control temperature unit, comprise spiral deflector in addition, the temperature of derivative solution effectively can be controlled by described control temperature unit, make the liquid in described reaction chamber form helical flow state by described spiral deflector, can effectively improve derivative efficiency.
By following description also by reference to the accompanying drawings, the present invention will become more clear, and these accompanying drawings are for explaining embodiments of the invention.
Accompanying drawing explanation
Fig. 1 is the column front derivation apparatus structure schematic diagram of liquid chromatography of the present invention.
Fig. 2 is the structural representation of the reaction unit of the column front derivation device of liquid chromatography as shown in Figure 1.
Fig. 3 is the structural representation of the temperature control panel of the column front derivation device of liquid chromatography as shown in Figure 1.
Fig. 4 is the circuit theory module map of the temperature control panel of the column front derivation device of liquid chromatography as shown in Figure 1.
Embodiment
With reference now to accompanying drawing, describe embodiments of the invention, element numbers similar in accompanying drawing represents similar element.As mentioned above, as Fig. 1, shown in 2, the column front derivation device 100 of the liquid chromatography that the embodiment of the present invention provides, comprise: the liquid solution 1 connected successively, pump 2, reaction unit 3, injector 4, insulation can chromatographic column 5, detecting device 6, described reaction unit 3 comprises housing 7, reaction chamber 8 and control temperature unit 9, described reaction chamber 8 is located in described housing 7 and one end and is communicated with described pump 2, the other end is communicated with described injector 4, and described reaction chamber 8 outer wall is provided with heat-insulation layer 10, described control temperature unit 9 comprises temperature control panel 91 and temperature-adjusting circuit plate 92, and described reaction chamber 8 bottom face is provided with one for holding the groove of described temperature control panel 91, described temperature control panel 91 to be fixed in described groove and to carry out temperature control to described reaction chamber 8, also comprise spiral deflector 11, it is inner that described spiral deflector 11 is located at described reaction chamber 8.Described heat-insulation layer 10 is asbestos material layer.
In an embodiment, as shown in Figure 2, bottom described reaction chamber 8 and top is respectively equipped with entrance 15 and the outlet 16 of liquid, and described entrance 15 is communicated with described pump 2, and described outlet 16 is communicated with described injector 4.By the effect of described spiral deflector 11, the reactant liquor of coming in from described entrance 15 will helically move upward by mode of motion, then flows out from described outlet 16.By described spiral deflector 11, reactant liquor can be made fully to mix.
In an embodiment, as shown in Figure 3, described temperature control panel 91 comprises rectangular-shaped main body sheet material, and described main body sheet material offers six grooves 910, and each groove 910 is fixed with a semiconductor chilling plate 17, and by these six described semiconductor chilling plates 17 and described reaction chamber 8 lower surface close contact, and the part of described reaction chamber 8 lower surface and described semiconductor chilling plate 17 close contact is the sheet metal that heat conductivility is good.
As in above-described embodiment, in six described semiconductor chilling plates 17, two groups of quantity often organized are divided into be three, first group is the one side and described reaction chamber 8 lower surface close contact that heat, second group is the one side and described reaction chamber 8 lower surface close contact of freezing, and first group of semiconductor chilling plate 17 and second group of spaced laying of semiconductor chilling plate 17.So, when needing to heat described reaction chamber 8, allow first group of semiconductor chilling plate 17 work, and second group of semiconductor chilling plate 17 does not work; When needing to freeze to described reaction chamber 8, allow second group of semiconductor chilling plate 17 work, and first group of semiconductor chilling plate 17 does not work.
In an embodiment, as shown in Figure 2, temperature sensing device 18 is also provided with in described reaction chamber 8.
As in above-described embodiment, as shown in Figure 4, also comprise control module 19, described temperature-adjusting circuit plate 92 and described temperature sensing device 18 are all connected with described control module 19, the temperature information that described control module 19 is fed back by described temperature sensing device 18, and then control described temperature-adjusting circuit plate 92 and work, and described temperature-adjusting circuit plate 92 to be located at described housing 7 inner.
In an embodiment, as shown in Figure 2, described housing 7 is also provided with air inlet 30 and air outlet 31, described air inlet 30 is located at described housing 7 upper surface, and described air outlet 31 is located at described housing 7 lower surface, and described air outlet 31 place is also provided with exhaust blower 32.
In an embodiment, described liquid solution 1 includes several different liquid solution, and be jointly communicated with described pump 2 by after various way solenoid valve 21, the flow velocity of described liquid solution 1 is by the power decision of described pump 2, and the flow velocity of solenoid valve to liquid solution of controllable flow speed size can be selected in addition to control.
Compared with prior art, composition graphs 1 ~ 4, in the column front derivation device 100 of liquid chromatography of the present invention, described control temperature unit 9 comprises temperature control panel 91 and temperature-adjusting circuit plate 92, and described reaction chamber 8 bottom face is provided with one for holding the groove of described temperature control panel 91, described temperature control panel 91 to be fixed in described groove and to carry out temperature control to described reaction chamber 8, makes the liquid in described reaction chamber 8 form helical flow state, can effectively improve derivative efficiency by described spiral deflector 11.
Above disclosedly be only the preferred embodiments of the present invention, certainly can not limit the interest field of the present invention with this, therefore according to the equivalent variations that the present patent application the scope of the claims is done, still belong to the scope that the present invention is contained.
Claims (8)
1. the column front derivation device of a liquid chromatography, it is characterized in that, comprise: the liquid solution connected successively, pump, reaction unit, injector, insulation can chromatographic column, detecting device, described reaction unit comprises housing, reaction chamber and control temperature unit, described reaction chamber is located in described housing and one end and is communicated with described pump, the other end is communicated with described injector, and described reacting outdoor wall is provided with heat-insulation layer, described control temperature unit comprises temperature control panel and temperature-adjusting circuit plate, and described reaction chamber bottom face is provided with one for holding the groove of described temperature control panel, described temperature control panel to be fixed in described groove and to carry out temperature control to described reaction chamber, also comprise spiral deflector, it is inner that described spiral deflector is located at described reaction chamber.
2. the column front derivation device of liquid chromatography as claimed in claim 1, it is characterized in that, bottom described reaction chamber and top is respectively equipped with entrance and the outlet of liquid, and described entrance is communicated with described pump, and described outlet is communicated with described injector.
3. the column front derivation device of liquid chromatography as claimed in claim 1, it is characterized in that, described temperature control panel comprises rectangular-shaped main body sheet material, and described main body sheet material is fixed with some semiconductor chilling plates, and by some described semiconductor chilling plates and described reaction chamber lower surface close contact, and the part of described reaction chamber lower surface and described semiconductor chilling plate close contact is the sheet metal that heat conductivility is good.
4. the column front derivation device of liquid chromatography as claimed in claim 3, it is characterized in that, in some described semiconductor chilling plates, be divided into two groups, first group is the one side and described reaction chamber lower surface close contact that heat, second group is the one side and described reaction chamber lower surface close contact of freezing, and first group of semiconductor chilling plate and second group of spaced laying of semiconductor chilling plate.
5. the column front derivation device of liquid chromatography as claimed in claim 4, is characterized in that, be also provided with temperature sensing device in described reaction chamber.
6. the column front derivation device of liquid chromatography as claimed in claim 5, it is characterized in that, also comprise control module, described temperature-adjusting circuit plate and described temperature sensing device are all connected with described control module, the temperature information that described control module is fed back by described temperature sensing device, and then control the work of described temperature-adjusting circuit plate.
7. the column front derivation device of liquid chromatography as claimed in claim 1, it is characterized in that, described housing is also provided with air inlet and air outlet, described air inlet is located at described housing upper surface, described air outlet is located at described housing lower surface, and described air outlet place is also provided with exhaust blower.
8. the column front derivation device of liquid chromatography as claimed in claim 6, it is characterized in that, be also provided with various way solenoid valve between described liquid solution and described pump, and described various way solenoid valve and described control module is electrically connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511031807.2A CN105486774B (en) | 2015-12-31 | 2015-12-31 | The column front derivation device of liquid chromatogram |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511031807.2A CN105486774B (en) | 2015-12-31 | 2015-12-31 | The column front derivation device of liquid chromatogram |
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| CN105486774A true CN105486774A (en) | 2016-04-13 |
| CN105486774B CN105486774B (en) | 2019-05-31 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1048333A1 (en) * | 1999-04-27 | 2000-11-02 | Metrohm Ag | Device and method for chemical derivatization |
| CN202119758U (en) * | 2011-05-30 | 2012-01-18 | 濮阳泓天威药业有限公司 | Oil bath type deriving reactor |
| CN102809622A (en) * | 2011-05-31 | 2012-12-05 | 湖北出入境检验检疫局检验检疫技术中心 | Special online derivatization device for bromate |
| CN103063785A (en) * | 2012-12-27 | 2013-04-24 | 大连依利特分析仪器有限公司 | Multi-functional pretreatment device used for amino acid analysis |
| CN204439602U (en) * | 2015-01-19 | 2015-07-01 | 天津出入境检验检疫局动植物与食品检测中心 | A kind of column front derivation device for liquid chromatography/chromatography of ions |
| CN205333578U (en) * | 2015-12-31 | 2016-06-22 | 华测检测认证集团股份有限公司 | Liquid chromatogram's pre -column device of deriving |
-
2015
- 2015-12-31 CN CN201511031807.2A patent/CN105486774B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1048333A1 (en) * | 1999-04-27 | 2000-11-02 | Metrohm Ag | Device and method for chemical derivatization |
| CN202119758U (en) * | 2011-05-30 | 2012-01-18 | 濮阳泓天威药业有限公司 | Oil bath type deriving reactor |
| CN102809622A (en) * | 2011-05-31 | 2012-12-05 | 湖北出入境检验检疫局检验检疫技术中心 | Special online derivatization device for bromate |
| CN103063785A (en) * | 2012-12-27 | 2013-04-24 | 大连依利特分析仪器有限公司 | Multi-functional pretreatment device used for amino acid analysis |
| CN204439602U (en) * | 2015-01-19 | 2015-07-01 | 天津出入境检验检疫局动植物与食品检测中心 | A kind of column front derivation device for liquid chromatography/chromatography of ions |
| CN205333578U (en) * | 2015-12-31 | 2016-06-22 | 华测检测认证集团股份有限公司 | Liquid chromatogram's pre -column device of deriving |
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| CN105486774B (en) | 2019-05-31 |
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Effective date of registration: 20180919 Address after: 100176 Beijing City Economic and Technological Development Zone, Chuang Chuang fourteen Street Huilong Sen science and Technology Park 21 building. Applicant after: China testing and Certification Group Beijing Co., Ltd. Address before: 518101 C, Hongwei Industrial Park, 70 District, Baoan District, Shenzhen, Guangdong. Applicant before: CENTRE TESTING INTERNATIONAL GROUP CO., LTD. |
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