CN201464435U - Fully-automatic device used for solid phase micro extraction and liquid chromatogram - Google Patents
Fully-automatic device used for solid phase micro extraction and liquid chromatogram Download PDFInfo
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- CN201464435U CN201464435U CN2009200875192U CN200920087519U CN201464435U CN 201464435 U CN201464435 U CN 201464435U CN 2009200875192 U CN2009200875192 U CN 2009200875192U CN 200920087519 U CN200920087519 U CN 200920087519U CN 201464435 U CN201464435 U CN 201464435U
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Abstract
The utility model relates to a fully-automatic device used for solid phase micro extraction and liquid chromatogram. The device comprises a first six-way valve and a second six-way valve which is connected with the first six-way valve through a connecting pipeline; a carrier fluid reagent bottle driven by a first driving pump, a quantification ring and an automatic sample introduction needle are connected on the first six-way valve; the second six-way valve is connected with a extraction column, a chromatographic column and a mobile phase reagent bottle driven by a second driving pump; and the outlet end of the chromatographic column is connected with a detector. The fully-automatic device has the advantages of simple structure and convenient operation; the sample introduction volume of the sample is accurately controlled by an automatic sample introduction device; the whole extraction and analysis processes both can be completed automatically under the control of programs; and the fully-automatic device not only ensures automatic operation, but also greatly improves the accuracy of the results measured.
Description
Technical field
The utility model relates to a kind of device that sample is carried out full-automatic pre-service and quantitative test, relates in particular to a kind of full-automatic solid-phase microextraction and liquid chromatography combined apparatus.
Background technology
Develop comparatively ripe today at multiple conventional analysis instrument and analytical approach, sample pretreatment still is considered to a process that takes time and effort, and may become the bottleneck that whole analysis task is finished smoothly even.At present, the robotization of sample pretreatment and high flux become the developing direction of modern analysis measuring technology.The chromatograph joint used automation equipment of solid-phase microextraction and gas phase has been realized commercialization, but the automation equipment of solid-phase microextraction and liquid chromatography coupling also seldom.1989, people such as Pawliszyn at first developed solid-phase microextraction (solid phase microextraction, SPME) technology.It has easy and simple to handle, and extraction does not need organic solvent fast, is easy to robotization, and the extraction efficiency height is conveniently with advantages such as gas chromatography, liquid chromatography couplings.Pawliszyn has proposed solid-phase microextraction in a kind of pipe-liquid chromatography coupling mode (in-tube SPME-HPLC).It adopts the quartz capillary of an inside coating to be the extraction part, be connected between an automatic sampler and the six-way valve, drive sample solution motion realization extraction repeatedly in kapillary with automatic sampler, with moving phase and appropriate solvent analyte desorption is analyzed in the quantitative ring of six-way valve then.This mode can realize the automatic operation of whole process by automatic sampler, but causes the quantitative result error owing to sample solution usually can be in automatic sampler mixes with the moving phase of remnants.
The utility model content
The purpose of this utility model is to address the above problem and provide a kind of simple in structure, and is easy to operate, when guaranteeing automation mechanized operation, can also improve the precision of measurement result greatly.
The utility model solves the problems of the technologies described above the technical scheme that is adopted:
It comprises first six-way valve and is attached thereto second six-way valve that connects by associated line, is connected with the transport fluid reagent bottle that drives through first infusion pump on described first six-way valve, also is connected with quantitative ring and auto injection pin on first six-way valve; The moving phase reagent bottle that described second six-way valve is connected with extraction column, chromatographic column and drives through second infusion pump, described chromatographic column endpiece links to each other with detecting device.
Also be provided with waste liquid outlet on the first above-mentioned six-way valve and second six-way valve.
Compared with prior art, the utility model has been obtained following technique effect:
1, this utility model can realize solid-phase microextraction and the full-automatic on-line coupling of liquid chromatography, and the volume of sample solution is accurately controlled by automatic sampler, and instrument makes up comparatively simple, easy to operate, can improve the precision of measurement greatly, the material of extraction usefulness can arbitrarily be changed, and bigger dirigibility is arranged;
2. this automation equipment can be realized the batch processing of a large amount of samples by programmed control, has alleviated operator's labour intensity greatly, also can improve the flux of sample preparation simultaneously.
3, by on first six-way valve and second six-way valve, also being provided with waste liquid outlet, make things convenient for it to clean, can further improve the precision of measurement device.
Description of drawings
Fig. 1 is the utility model planar structure synoptic diagram;
Fig. 2 is for using eight kinds of chromatograms that the sulfamido microbiotic obtains in the utility model analysis water-like.
Wherein: 1-transport fluid reagent bottle, 2-first infusion pump, 3-first six-way valve, 4-quantitatively encircle, 5-auto injection pin, 6-waste liquid outlet, 7-associated line, 8-extraction column, 9-second six-way valve, 10-moving phase reagent bottle, 11-second infusion pump, 12-chromatographic column, 13-detecting device.
Embodiment
Further specify embodiment of the present utility model below in conjunction with accompanying drawing.
Embodiment 1
Referring to Fig. 1, a kind of full-automatic solid-phase microextraction and liquid chromatography combined apparatus, it comprises first six-way valve 3 and is attached thereto second six-way valve 9 that connects by associated line 7, be connected with on described first six-way valve on transport fluid reagent bottle 1, the first six-way valve that first infusion pump 2 drives and also be connected with quantitative ring 4 and auto injection pin 5; The moving phase reagent bottle 10 that described second six-way valve is connected with extraction column 8, chromatographic column 12 and drives through second infusion pump 11, the described chromatographic column other end links to each other with detecting device 13.On described first six-way valve and second six-way valve, also be provided with waste liquid outlet 6, make things convenient for the cleaning of device like this, can reduce of the influence of the residuum of device inside measurement result.
The step of using the utility model to analyze is:
Activation: transport fluid reagent bottle 1 is equipped with transport fluid, drives through first infusion pump 2, when first six-way valve 3 is in load sample (LOAD) position (solid line among the figure), transport fluid is passed through the extraction kapillary with required flow rate, and it is activated.
Extraction: auto injection pin 5 injects sample loop with the sample solution of certain volume, and the six-way valve of automatic sampler switches to sample introduction (INJECT) position (dotted line among the figure).Transport fluid drives sample solution and enters extraction column from sample loop, begins extraction.
Clean: after extraction was finished, transport fluid still kept being replaced by it by the sample solution of extraction column in pipe, thereby prevents that the analyte that is not adsorbed from entering chromatographic column and causing quantitative error.
Desorb: second six-way valve 9 switches to sample introduction (INJECT) position, make moving phase through the extraction kapillary with absorption analyte desorption on chromatographic column.
Analyze: after desorb finishes, second six-way valve 9 is switched to load sample (LOAD) position, the moving phase in the moving phase reagent bottle 10 is driven by second infusion pump 11, enters detecting device 13 through chromatographic column 12, carries out chromatographic resolution and detection.
Whole extraction, analytic process comprises that the variation of first infusion pump and the second infusion pump flow velocity and the switching of first six-way valve and second six-way valve all can be finished automatically by software control, concrete software those skilled in the art are specific design as required, this auto-control software is a common practise in the society of modern automation, does not just do concrete description at this.Every commercialization instrument of being furnished with automatic sampling apparatus and flow channel switching valve (as above-mentioned six-way valve) through after the above repacking, all can be realized the solid-phase microextraction and the liquid chromatography coupling of robotization.
For the ease of understanding the utility model, the applicant provides an automatic control program table.Simultaneously, the first above-mentioned infusion pump and second infusion pump are represented with pump A and pump B respectively hereinafter; First six-way valve and second six-way valve are represented with transfer valve A and transfer valve B respectively.
Table 1: the control program table of full-automatic solid-phase microextraction liquid chromatography coupling
With solid-phase microextraction in managing and high performance liquid chromatography on-line coupling, eight kinds of sulfamido microbiotic are that example illustrates result of use of the present invention in the automatical analysis water sample below.It is 1. sulphadiazines (SDZ), 2. sulfapryidine (SPD), 3. sulfamethyldiazine (SMR), 4. sulfanilamide (SN) is to methoxy pyrimidine (SME), 5. sulfadimidine (SMZ), 6. daimeton (SMM), 7. cistosulfa (SCP), 8. fanasil (SD).
Efficient liquid phase chromatographic analysis condition: with Hypersil ODS post (200mm * 4.6mm i.d.; 5 μ m) be analytical column, i.e. the carbon 18 bonded silica gel posts of U.S. power ﹠ light company, length 200mm, internal diameter 4.6mm, packing material size 5 μ m.Moving phase is that volume ratio is acetonitrile/20 mM ammonium acetate buffer solutions of 24: 76, and buffer solution pH is 5.0, and flow velocity 0.8mL/min, ultraviolet detection wavelength are 269nm, 30 ℃ of column temperatures.Solid-phase microextraction condition in the pipe: extraction column is for containing octyl group and sulfonic internal diameter is 0.25mm, and length is the monolithic silica column of 150mm, and the transport fluid percent by volume is 0.2% aqueous formic acid, carries out desorb with moving phase.
Analytic process: with eight kinds of sulfamido microbiotic standard solution percent by volumes is 0.2%, and the formic acid solution dilution obtains the 50ng/mL test solution.After solid-phase microextraction, with concentration water sample direct injected peak area ratio, eight kinds of sulfamido microbiotic obtain obvious enrichment.
Referring to Fig. 2, it is the chromatogram comparison diagram before and after the 50ng/mL water sample solid-phase microextraction.A is the chromatogram of 20 μ L water sample (50ng/mL) direct injected, and B is the chromatograms of 300 μ L water samples (50ng/mL) after the solid-phase microextraction enrichment.Chromatographic peak: 21. sulphadiazines (SDZ), 22. sulfapryidine (SPD), 23. sulfamethyldiazine (SMR), 24. sulfanilamide (SN) is to methoxy pyrimidine (SME), 25. sulfadimidine (SMZ), 26. daimeton (SMM), 27. cistosulfas (SCP), 28. fanasils (SD).
The result shows use solid-phase microextraction provided by the invention and liquid chromatography on-line coupling device automatical analysis sample, concentration effect is obvious. and we have examined or check the reappearance that this automation equipment extracts analysis, concrete experimental data sees Table the relative standard deviation (RSD)＜0.5% that the retention time that obtains is analyzed in 2. 8 extractions, the comparison with standard deviation (RSD)＜5.4% of peak area, this solid-phase extraction device precision height is described, favorable reproducibility, reliable results, satisfy the needs of routine analysis fully. in addition, this automation equipment can be realized the batch processing of a large amount of samples by program, alleviate operator's labour intensity greatly, also can improve the flux of sample preparation simultaneously.
Table 2: eight kinds of sulfa drugss full-automatic retention time and peak areas that online solid-phase microextraction-the liquid chromatography ultraviolet detection obtains
Protection domain of the present utility model is not limited to the above embodiments, and obviously, those skilled in the art can carry out various changes and distortion and not break away from scope and spirit of the present utility model the utility model.If these changes and distortion belong in the scope of the utility model claim and equivalent technologies thereof, intention then of the present utility model also comprises these changes and is out of shape interior.
Claims (2)
1. full-automatic solid-phase microextraction and liquid chromatography combined apparatus, it is characterized in that: it comprises first six-way valve (3) and second six-way valve (9) that is attached thereto by associated line (7), be connected with the transport fluid reagent bottle (1) that drives through first infusion pump (2) on described first six-way valve, also be connected with quantitative ring (4) and auto injection pin (5) on first six-way valve; The moving phase reagent bottle (10) that described second six-way valve is connected with extraction column (8), chromatographic column (12) and drives through second infusion pump (11), described chromatographic column endpiece links to each other with detecting device (13).
2. full-automatic solid-phase microextraction according to claim 1 and liquid chromatography combined apparatus is characterized in that: also be provided with waste liquid outlet (6) on described first six-way valve and second six-way valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009200875192U CN201464435U (en) | 2009-07-24 | 2009-07-24 | Fully-automatic device used for solid phase micro extraction and liquid chromatogram |
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| CN2009200875192U CN201464435U (en) | 2009-07-24 | 2009-07-24 | Fully-automatic device used for solid phase micro extraction and liquid chromatogram |
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| CN201464435U true CN201464435U (en) | 2010-05-12 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302887A (en) * | 2011-08-15 | 2012-01-04 | 西北核技术研究所 | High-efficient pressurizing and sample-introducing device for preparative gas chromatography |
| CN103278590A (en) * | 2013-05-07 | 2013-09-04 | 大连依利特分析仪器有限公司 | Integrated automatic sampling fraction collector |
| CN110095549A (en) * | 2019-06-12 | 2019-08-06 | 吉林省产品质量监督检验院(吉林省农产品认证中心) | The detection device and method of aflatoxin in a kind of Grain and its product |
| CN113358767A (en) * | 2021-04-30 | 2021-09-07 | 上海睿康生物科技有限公司 | Full-automatic ultra-high performance liquid chromatography tandem mass spectrometry detection system and working method |
-
2009
- 2009-07-24 CN CN2009200875192U patent/CN201464435U/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302887A (en) * | 2011-08-15 | 2012-01-04 | 西北核技术研究所 | High-efficient pressurizing and sample-introducing device for preparative gas chromatography |
| CN103278590A (en) * | 2013-05-07 | 2013-09-04 | 大连依利特分析仪器有限公司 | Integrated automatic sampling fraction collector |
| CN110095549A (en) * | 2019-06-12 | 2019-08-06 | 吉林省产品质量监督检验院(吉林省农产品认证中心) | The detection device and method of aflatoxin in a kind of Grain and its product |
| CN113358767A (en) * | 2021-04-30 | 2021-09-07 | 上海睿康生物科技有限公司 | Full-automatic ultra-high performance liquid chromatography tandem mass spectrometry detection system and working method |
| CN113358767B (en) * | 2021-04-30 | 2023-04-07 | 上海睿康生物科技有限公司 | Full-automatic ultra-high performance liquid chromatography tandem mass spectrometry detection system and working method |
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| C14 | Grant of patent or utility model | ||
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Owner name: BEIJING HIGHSIGHT TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: WUHAN UNIVERSITY Effective date: 20110526 |
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| C41 | Transfer of patent application or patent right or utility model | ||
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Free format text: CORRECT: ADDRESS; FROM: 430072 LUOJIASHAN, WUCHANG, WUHAN CITY, HUBEI PROVINCE TO: 100191 ROOM 302,MUDAN VENTURE BUILDING, NO. 2, HUAYUAN ROAD, HAIDIAN DISTRICT, BEIJING |
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| TR01 | Transfer of patent right |
Effective date of registration: 20110526 Address after: 100191, room 2, peony building, No. 302 peony, Haidian District, Beijing, Huayuan Road Patentee after: Beijing constant love Kang Technology Development Co., Ltd. Address before: 430072 Hubei city of Wuhan province Wuchang Luojiashan Patentee before: Wuhan University |
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| ASS | Succession or assignment of patent right |
Owner name: WEITAIKE TECHNOLOGY (WUHAN) CO., LTD. Free format text: FORMER OWNER: BEIJING HIGHSIGHT TECHNOLOGY CO., LTD. Effective date: 20111231 |
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Free format text: CORRECT: ADDRESS; FROM: 100191 HAIDIAN, BEIJING TO: 430074 WUHAN, HUBEI PROVINCE |
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| TR01 | Transfer of patent right |
Effective date of registration: 20111231 Address after: 430074, Hubei East Lake Development Zone, hi tech Avenue, No. 666, Wuhan National Bio industrial base project B, C, D District, R & D building, B1 building, Wuhan Patentee after: Vitec Technology (Wuhan) Co. Ltd. Address before: 100191, room 2, peony building, No. 302 peony, Haidian District, Beijing, Huayuan Road Patentee before: Beijing constant love Kang Technology Development Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
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| EXPY | Termination of patent right or utility model |