CN204017444U - A kind of efficient magnetic control disperses solid-phase extraction device - Google Patents
A kind of efficient magnetic control disperses solid-phase extraction device Download PDFInfo
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技术领域technical field
本实用新型属于固相萃取技术领域,涉及一种样品分析预处理设备,尤其涉及一种高效磁控分散固相萃取装置,用于分散固相萃取时磁性吸附材料的均匀分散、吸附脱附及固/液两相的快速分离。The utility model belongs to the technical field of solid phase extraction, and relates to a sample analysis pretreatment device, in particular to a high-efficiency magnetic control dispersion solid phase extraction device, which is used for uniform dispersion, adsorption and desorption of magnetic adsorption materials during dispersive solid phase extraction. Rapid separation of solid/liquid two phases.
背景技术Background technique
由于分析样品基质的复杂性,新型高效的样品前处理技术的研究显得尤为重要。分散固相萃取技术是近年来快速发展而来的一种富集和净化的样品预处理技术,但由于传统分散固相萃取技术存在操作过程繁琐、处理时间长和固液分离困难等不足而受到限制。磁分离的历史最早可以追溯到100多年前,1865年Porter首次将其应用到大规模的水处理设备中。后来逐渐应用到微生物学、细胞生物学、分子生物学和生物化学、分析化学以及生物技术和环保技术等领域。基于物理吸附过程的差异,磁分离主要分为:直接磁分离,加入絮凝剂的磁分离,应用磁性吸附剂的分离(即磁控固相萃取),以及与其它过程结合的磁分离四种形式。磁控固相萃取的基本原理是利用目标物在磁性吸附材料与溶液之间的两相分配,当样品溶液与磁性吸附剂相接触时,通过选择性吸附,可以实现对目标分析物的富集及其与共存组分的分离,然后采用磁控技术将固/液两相分离。磁固相萃取的模式按照固定相的存在形式,可以分为分散式和填充柱式两种。其中分散式多在烧杯中进行,在超声分散纳米磁性颗粒后,通过外加磁场可使上层溶液迅速澄清,并实现批操作,在萃取过程中,当磁性材料被加入到含有目标分析物的溶液中时,目标分析物就被选择性地吸附在磁性材料上,外加磁场后,吸附了目标分析物的磁性材料与原溶液快速分离。随后,采用适宜的溶剂将目标分析物从纳米磁性材料上洗脱下来,从而实现对目标分析物的纯化和富集,最后将洗脱液引入后续的分析仪器进行检测。Due to the complexity of the analysis sample matrix, the research of new and efficient sample pretreatment technology is particularly important. Dispersive solid phase extraction technology is a kind of enrichment and purification sample pretreatment technology developed rapidly in recent years. limit. The history of magnetic separation can be traced back more than 100 years ago. In 1865, Porter first applied it to large-scale water treatment equipment. Later, it was gradually applied to the fields of microbiology, cell biology, molecular biology and biochemistry, analytical chemistry, biotechnology and environmental protection technology. Based on the difference in the physical adsorption process, magnetic separation is mainly divided into four forms: direct magnetic separation, magnetic separation with flocculant added, separation with magnetic adsorbent (ie magnetic control solid phase extraction), and magnetic separation combined with other processes. . The basic principle of magnetically controlled solid-phase extraction is to use the two-phase distribution of the target substance between the magnetic adsorption material and the solution. When the sample solution is in contact with the magnetic adsorbent, the enrichment of the target analyte can be achieved through selective adsorption. And its separation from the coexisting components, and then the solid/liquid two phases are separated by magnetic control technology. According to the existence form of the stationary phase, the magnetic solid phase extraction mode can be divided into two types: dispersed type and packed column type. Among them, the dispersion method is mostly carried out in a beaker. After ultrasonically dispersing the nano-magnetic particles, the upper solution can be clarified quickly by applying an external magnetic field, and batch operation can be realized. During the extraction process, when the magnetic material is added to the solution containing the target analyte , the target analyte is selectively adsorbed on the magnetic material, and after an external magnetic field is applied, the magnetic material adsorbed by the target analyte is rapidly separated from the original solution. Subsequently, the target analyte is eluted from the nano-magnetic material with a suitable solvent, thereby realizing the purification and enrichment of the target analyte, and finally the eluate is introduced into a subsequent analysis instrument for detection.
经查,现有专利号为CN201220351885.6的中国专利《磁控磁性基质固相萃取装置》,柱体上端有上口,下端有漏斗形下口,主体呈圆筒形,柱体外套有线圈和线圈骨架,线圈的端线串联有直流电源、开关和滑动变阻器。通过外加磁场产生磁性定向移动作用,使磁性样品在顺磁方向下加快萃取速度,克服了实验过程中萃取缓慢、不完全的缺点,节省了时间。但是它的磁性吸附剂是作为固体基质通过筛板填充在柱体内,在萃取时,磁性吸附剂是固定的,在样品溶液中不能充分分散,因此存在萃取效率低的缺陷,需要进一步改进,使磁性吸附剂在样品溶液中可进行均匀分散与吸附,实现固/液两相的快速磁分离,提高萃取效率。After investigation, the existing patent No. CN201220351885.6 is the Chinese patent "Magnetic Control Magnetic Matrix Solid-Phase Extraction Device". The upper end of the column has an upper opening, and the lower end has a funnel-shaped lower opening. and the coil frame, and the terminal wire of the coil is connected in series with a DC power supply, a switch and a sliding rheostat. The magnetic directional movement is generated by an external magnetic field, so that the extraction speed of the magnetic sample is accelerated in the paramagnetic direction, which overcomes the shortcomings of slow and incomplete extraction during the experiment and saves time. However, its magnetic adsorbent is filled in the column as a solid matrix through a sieve plate. During extraction, the magnetic adsorbent is fixed and cannot be fully dispersed in the sample solution. Therefore, there is a defect of low extraction efficiency, which needs further improvement. The magnetic adsorbent can be uniformly dispersed and adsorbed in the sample solution to realize the rapid magnetic separation of solid/liquid two phases and improve the extraction efficiency.
实用新型内容Utility model content
本实用新型所要解决的技术问题是提供一种集超声吸附、净化、洗脱和固/液两相磁分离于一体的高效磁控分散固相萃取装置,具有操作简单、萃取效率高的特点。The technical problem to be solved by the utility model is to provide a high-efficiency magnetic control dispersion solid-phase extraction device integrating ultrasonic adsorption, purification, elution and solid/liquid two-phase magnetic separation, which has the characteristics of simple operation and high extraction efficiency.
本实用新型为解决上述技术问题所采用的技术方案为:一种高效磁控分散固相萃取装置,其特征在于:包括若干个相互并联设置的可同时进行批量处理样品的萃取柱柱体,萃取柱柱体的上端设有进样口,下端设有出样口,萃取柱柱体内装有磁性微米吸附剂,在萃取柱柱体内的底部设有筛板,筛板上设有超声片,萃取柱柱体外绕有线圈,线圈的端线与电源、电源开关和滑动变阻器相串联。The technical scheme adopted by the utility model to solve the above technical problems is: a high-efficiency magnetic control dispersion solid-phase extraction device, which is characterized in that it includes several extraction columns arranged in parallel and can process samples in batches at the same time. The upper end of the column body is provided with a sample inlet, and the lower end is provided with a sample outlet. The extraction column body is equipped with a magnetic micron adsorbent, and the bottom of the extraction column body is equipped with a sieve plate. The sieve plate is equipped with an ultrasonic sheet. A coil is wound outside the column, and the end wire of the coil is connected in series with the power supply, the power switch and the sliding rheostat.
作为改进,所述的线圈为半环线圈,绕在萃取柱柱体外的线圈骨架上,萃取柱柱体呈透明状或者在萃取柱柱体上设有纵向透明窗,在萃取柱柱体的外表面或透明窗上设有可显示溶液体积的刻度。As an improvement, the coil is a half-ring coil wound on the coil skeleton outside the extraction column body, the extraction column body is transparent or a longitudinal transparent window is provided on the extraction column body, and There is a scale on the surface or a transparent window that can display the volume of the solution.
作为改进,所述萃取柱柱体的下端出样口呈漏斗状并设置有控制阀。As an improvement, the sample outlet at the lower end of the extraction column body is funnel-shaped and provided with a control valve.
作为改进,所述萃取柱柱体为1~36个。As an improvement, there are 1 to 36 extraction columns.
再改进,所述萃取柱柱体为1个、6个或12个。As a further improvement, there are 1, 6 or 12 extraction columns.
与现有技术相比,本实用新型的优点在于:设有多个萃取柱柱体,可单个或多个同时批量处理样品,萃取柱柱体表面的刻度可以准确量取待处理样品的体积,底部的超声片能保证磁性吸附剂在样品溶液中均匀分散与吸附,出样口处的控制阀能方便地控制磁性吸附剂与样品溶液的接触时间;工作时,通电线圈所产生的磁场使每个柱体中吸附有目标分析物的磁性微米吸附剂在该外加磁场作用下表现一定的磁化强度,产生磁场力,从而实现固/液两相的快速磁分离;半环线圈匝数可根据实际需要进行增减,磁场力大小可通过调节滑动变阻器以控制电流大小实现。本实用新型克服了传统分散固相萃取技术操作繁琐、重现性差、萃取缓慢和萃取效率低的缺点,本实用新型集超声吸附、净化、洗脱和固/液两相磁分离于一体,具有操作简单、萃取速度快、效率高的特点。Compared with the prior art, the utility model has the advantages that multiple extraction columns are provided, and samples can be processed in batches at the same time, one or more, and the scale on the surface of the extraction column can accurately measure the volume of the sample to be processed. The ultrasonic sheet at the bottom can ensure the uniform dispersion and adsorption of the magnetic adsorbent in the sample solution, and the control valve at the sample outlet can conveniently control the contact time between the magnetic adsorbent and the sample solution; when working, the magnetic field generated by the energized coil makes each The magnetic micro-adsorbent adsorbed with the target analyte in each column exhibits a certain magnetization intensity under the action of the external magnetic field, generating a magnetic field force, thereby realizing the rapid magnetic separation of the solid/liquid two-phase; the number of turns of the half-ring coil can be determined according to the actual situation It needs to be increased or decreased, and the magnitude of the magnetic field force can be realized by adjusting the sliding rheostat to control the magnitude of the current. The utility model overcomes the shortcomings of traditional dispersive solid-phase extraction technology, such as cumbersome operation, poor reproducibility, slow extraction and low extraction efficiency. The utility model integrates ultrasonic adsorption, purification, elution and solid/liquid two-phase magnetic separation, and has the advantages of It has the characteristics of simple operation, fast extraction speed and high efficiency.
附图说明Description of drawings
图1是本实用新型专利所涉及装置的结构示意图;Fig. 1 is a schematic structural view of the device involved in the utility model patent;
图2是图1中单个萃取柱的结构示意图。Fig. 2 is a schematic structural view of a single extraction column in Fig. 1 .
具体实施方式Detailed ways
以下结合附图实施例对本实用新型专利作进一步详细描述。Below in conjunction with accompanying drawing embodiment, the utility model patent is described in further detail.
如图1、2所示,本实施例的高效磁控分散固相萃取装置,包括6个相互并联设置的可同时进行批量处理样品的萃取柱柱体1,萃取柱柱体1的上端设有进样口11,下端设有出样口,萃取柱柱体1外设有线圈骨架6,线圈骨架6上绕有线圈3,每个萃取柱柱体1外的线圈3互相串联,线圈3的端线与电源9、电源开关10和滑动变阻器8相串联构成控制回路;萃取柱柱体1内装有磁性微米吸附剂7,在萃取柱柱体1内的底部设有筛板5,筛板5上设有超声片4,超声片4的存在能使磁性微米吸附剂7在样品溶液中实现超声辅助均匀分散,线圈3为半环线圈,萃取柱柱体1为透明状,在萃取柱柱体1的外表面设有可显示溶液体积的刻度,这样能准确量取液体样品的体积;萃取柱柱体1的下端出样口呈漏斗状并设置有控制阀2,能方便控制磁性吸附剂与样品溶液的接触时间。As shown in Figures 1 and 2, the high-efficiency magnetic control dispersive solid-phase extraction device of the present embodiment includes 6 extraction columns 1 that are arranged in parallel and can simultaneously process samples in batches. The upper end of the extraction column 1 is provided with The sample inlet 11 is provided with a sample outlet at the lower end, and a coil bobbin 6 is arranged outside the column body 1 of the extraction column, and a coil 3 is wound on the frame body 6, and the coils 3 outside the column body 1 of each extraction column are connected in series, and the coils 3 are connected in series. The terminal line is connected in series with the power supply 9, the power switch 10 and the sliding rheostat 8 to form a control loop; the extraction column body 1 is equipped with a magnetic micron adsorbent 7, and the bottom of the extraction column body 1 is provided with a sieve plate 5, and on the sieve plate 5 An ultrasonic sheet 4 is provided. The presence of the ultrasonic sheet 4 enables the magnetic micro-adsorbent 7 to achieve ultrasonic-assisted uniform dispersion in the sample solution. The coil 3 is a semi-circular coil, and the extraction column body 1 is transparent. The outer surface of the extraction column is provided with a scale that can display the volume of the solution, so that the volume of the liquid sample can be accurately measured; the sample outlet at the lower end of the extraction column body 1 is funnel-shaped and is provided with a control valve 2, which can facilitate the control of the magnetic adsorbent and the sample. solution contact time.
下面通过实施例对本实用新型专利的工作状态做进一步说明。The working status of the utility model patent will be further described below by way of examples.
实施例1Example 1
1、分散与吸附:电源开关10处于断开,线圈3未通电,出样口处控制阀2闭合,运行超声片4,此时磁性吸附剂7在样品溶液中充分分散,并吸附溶液中的杂质。1. Dispersion and adsorption: The power switch 10 is off, the coil 3 is not powered, the control valve 2 at the sample outlet is closed, and the ultrasonic sheet 4 is operated. At this time, the magnetic adsorbent 7 is fully dispersed in the sample solution and absorbs the Impurities.
2、磁分离:待充分吸附后,闭合电源开关10,此时线圈3开始通电并产生磁场,打开出样口控制阀2,收集经吸附杂质后的液体样品,磁性微米吸附剂7在磁场力作用下实现有效的固/液两相磁分离。2. Magnetic separation: After fully adsorbing, close the power switch 10, at this time the coil 3 starts to energize and generate a magnetic field, open the sample outlet control valve 2, and collect the liquid sample after absorbing impurities. Effective solid/liquid two-phase magnetic separation is realized under the action.
3、目标物的浓缩:收集溶液,氮吹浓缩,定容后按需求进行定性定量分析。3. Concentration of the target object: collect the solution, blow it with nitrogen and concentrate it, and conduct qualitative and quantitative analysis according to the requirements after constant volume.
实施例2Example 2
1、分散与吸附:电源开关10处于断开,线圈3未通电,出样口处控制阀2闭合,运行超声片4,此时磁性吸附剂7在样品溶液中充分分散,并吸附目标物。1. Dispersion and adsorption: The power switch 10 is off, the coil 3 is not energized, the control valve 2 at the sample outlet is closed, and the ultrasonic sheet 4 is operated. At this time, the magnetic adsorbent 7 is fully dispersed in the sample solution and adsorbs the target.
2、磁分离:待充分吸附后,闭合电源开关10,此时线圈3开始通电并产生磁场,打开出样口控制阀2,丢弃经吸附后的液体样品,磁性微米吸附剂7在磁场力作用下实现有效的固/液两相磁分离。2. Magnetic separation: After fully adsorbed, close the power switch 10, at this time the coil 3 starts to energize and generate a magnetic field, open the sample outlet control valve 2, and discard the adsorbed liquid sample, the magnetic micron adsorbent 7 is under the action of the magnetic field effective solid/liquid two-phase magnetic separation.
3、淋洗:关闭出样口控制阀2,断开电源开关10,从萃取柱柱体1上端进样口11加入杂质淋洗液,运行超声片4,使淋洗液与磁性微米吸附剂7充分接触,待一段时间后,闭合电源开关10,体系产生磁场,开启出样口控制阀2,通过出样口舍弃杂质淋洗液。3. Rinse: close the sample outlet control valve 2, disconnect the power switch 10, add impurity eluent from the upper end of the extraction column column body 1, and add impurity eluent, and run the ultrasonic film 4 to make the eluent and magnetic micron adsorbent 7 Fully contact, after a period of time, close the power switch 10, the system generates a magnetic field, open the sample outlet control valve 2, and discard the impurity eluent through the sample outlet.
4、目标物的洗脱与浓缩:关闭出样口控制阀2,断开电源开关10,从萃取柱柱体1上端进样口11加入目标物洗脱液,运行超声片4,使目标物洗脱液与磁性微米吸附剂7充分接触,目标分析物被洗脱,此时闭合电源开关10,体系产生磁场,开启出样口控制阀2,收集洗脱液,氮吹浓缩,定容后按需求进行定性定量分析。4. The elution and concentration of the target substance: close the sample outlet control valve 2, disconnect the power switch 10, add the target substance eluent from the injection port 11 at the upper end of the extraction column body 1, run the ultrasonic film 4, and make the target substance The eluent is in full contact with the magnetic micron adsorbent 7, and the target analyte is eluted. At this time, the power switch 10 is closed, the system generates a magnetic field, the control valve 2 of the sample outlet is opened, the eluent is collected, concentrated by nitrogen blowing, and after constant volume Qualitative and quantitative analysis as required.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2018129789A1 (en) * | 2017-01-11 | 2018-07-19 | 中国科学院过程工程研究所 | Whole-process continuous gas-assisted magnetic separation system |
| CN108760425A (en) * | 2018-05-30 | 2018-11-06 | 重庆第二师范学院 | A kind of graphite oxide alkenyl pretreating device and its application in food inspection |
| CN108939613A (en) * | 2018-07-19 | 2018-12-07 | 贵州省人民医院 | Eucommia ulmoides extracts high-efficiency device for extracting and method for Prevention of cardiovascular disease |
| CN109073518A (en) * | 2016-04-01 | 2018-12-21 | 多伦多大学管理委员会 | The DMF method and system being concentrated into analyte from large volume using magnetic particle in smaller size smaller |
| CN110508030A (en) * | 2019-09-18 | 2019-11-29 | 深圳市易瑞生物技术股份有限公司 | A kind of Magnetic solid phases extraction column and its application method |
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| CN109073518A (en) * | 2016-04-01 | 2018-12-21 | 多伦多大学管理委员会 | The DMF method and system being concentrated into analyte from large volume using magnetic particle in smaller size smaller |
| CN109073518B (en) * | 2016-04-01 | 2020-02-28 | 多伦多大学管理委员会 | DMF method and system for concentrating analytes from large volumes to smaller volumes using magnetic particles |
| US10976225B2 (en) | 2016-04-01 | 2021-04-13 | The Governing Council Of The University Of Toronto | DMF method and system for concentrating analyte from large volumes into smaller volumes using magnetic microparticles |
| WO2018129789A1 (en) * | 2017-01-11 | 2018-07-19 | 中国科学院过程工程研究所 | Whole-process continuous gas-assisted magnetic separation system |
| CN108760425A (en) * | 2018-05-30 | 2018-11-06 | 重庆第二师范学院 | A kind of graphite oxide alkenyl pretreating device and its application in food inspection |
| CN108939613A (en) * | 2018-07-19 | 2018-12-07 | 贵州省人民医院 | Eucommia ulmoides extracts high-efficiency device for extracting and method for Prevention of cardiovascular disease |
| CN108939613B (en) * | 2018-07-19 | 2020-08-11 | 贵州省人民医院 | Eucommia ulmoides extract efficient extraction device and method for preventing and treating cardiovascular diseases |
| CN110508030A (en) * | 2019-09-18 | 2019-11-29 | 深圳市易瑞生物技术股份有限公司 | A kind of Magnetic solid phases extraction column and its application method |
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