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CN101620041B - Automatic flow-path separation device - Google Patents

Automatic flow-path separation device Download PDF

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Publication number
CN101620041B
CN101620041B CN2009100900682A CN200910090068A CN101620041B CN 101620041 B CN101620041 B CN 101620041B CN 2009100900682 A CN2009100900682 A CN 2009100900682A CN 200910090068 A CN200910090068 A CN 200910090068A CN 101620041 B CN101620041 B CN 101620041B
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way valve
bottle
separation
collector
pipeline
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CN101620041A (en
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李重九
马晓东
韩天祥
李西恭
李晓娟
张新忠
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China Agricultural University
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China Agricultural University
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Abstract

本发明涉及一种自动分离流路装置,它包括依次通过管路相互连接的一溶剂瓶、一输液泵、一六通阀、一分离元件、一收集器,一样品瓶、一柱塞泵和一废液瓶,其特征在于:它包括两个三通阀;第一个所述三通阀的三个端口分别通过管路连接所述溶剂瓶、六通阀和柱塞泵;第二个所述三通阀的三个端口分别通过管路连接所述收集器、分离元件和废液瓶;所述六通阀通过一管路直接连接所述收集器。本发明仅设置了两个三通阀,与已有的分离流路装置相比,结构简单,成本降低,通过控制两个三通阀与一个六通阀的切换,对柱塞泵和采样收集器进行控制,同样自动完成了样品的定量取样、清洗、样品分离、收集、丢弃五个过程。本发明提高了重复精度,降低了仪器生产成本和日常维护难度。

The invention relates to an automatic separation flow path device, which comprises a solvent bottle, an infusion pump, a six-way valve, a separation element, a collector, a sample bottle, a plunger pump and A waste liquid bottle is characterized in that: it comprises two three-way valves; the three ports of the first three-way valve are respectively connected to the solvent bottle, the six-way valve and the plunger pump through pipelines; the second The three ports of the three-way valve are respectively connected to the collector, the separation element and the waste liquid bottle through pipelines; the six-way valve is directly connected to the collector through a pipeline. Only two three-way valves are provided in the present invention. Compared with the existing separation flow device, the structure is simple and the cost is reduced. By controlling the switching between two three-way valves and one six-way valve, the plunger pump and sampling It also automatically completes the five processes of quantitative sampling, cleaning, sample separation, collection and discarding of samples. The invention improves the repetition accuracy, reduces the production cost of the instrument and the difficulty of daily maintenance.

Description

一种自动分离流路装置An automatic separation flow path device

技术领域technical field

本发明涉及一种生物或化学样品分离、制备等过程中使用的分离流路装置,特别是关于一种自动分离流路装置。The invention relates to a separation flow device used in the separation and preparation of biological or chemical samples, in particular to an automatic separation flow device.

背景技术Background technique

现有的普通分离流路装置(以色谱仪为例,如图1所示)主要包括依次连接的溶剂瓶1、输液管2、输液泵3、输液管4、六通阀5、输液管6、分离元件7(色谱柱)、输液管8、检测器9、输液管10、收集器11,以及样品瓶12等。分析过程中,进样、收集一般是靠手工进行繁琐的操作,分析效率低,且重复精度受实验员操作熟练程度的影响。而现有的自动分离流路装置结构复杂。The existing common separation flow device (take the chromatograph as an example, as shown in Figure 1) mainly includes a solvent bottle 1, an infusion tube 2, an infusion pump 3, an infusion tube 4, a six-way valve 5, and an infusion tube 6 connected in sequence. , separation element 7 (chromatographic column), infusion tube 8, detector 9, infusion tube 10, collector 11, and sample bottle 12, etc. During the analysis process, sample injection and collection are generally cumbersome operations by hand, the analysis efficiency is low, and the repeatability is affected by the operator's proficiency. However, the existing automatic separation flow path device has a complex structure.

本申请人于2005年10月25日提出了一种名称为“一种自动分离流路装置”,专利申请号为:200510114554.5的发明专利,其是在现有手工操作的基础上进行了改进(如图2所示),其除包括现有技术的溶剂瓶1、输液管2、输液泵3、输液管4、六通阀5、输液管6、分离元件7(色谱柱)、输液管8、检测器9、输液管10、收集器11和样品瓶12以外,主要特征是增加了三个三通阀21、22、23一个柱塞泵24,电动控制装置,同时收集器11是兼具采样和收集于一身的采样收集器11。该发明专利申请可以自动完成样品的定量取样、清洗、样品分离、收集、丢弃这五个过程,克服了现有技术中繁琐的手工操作。但是由于其中包括了三个分别通过管路连接六通阀5的三通阀21、22、23,因此仪器的制造成本较高,结构较复杂,维护也有一定困难。On October 25, 2005, the applicant proposed an invention patent named "an automatic separation flow path device" with the patent application number: 200510114554.5, which was improved on the basis of the existing manual operation ( As shown in Figure 2), it except comprises prior art solvent bottle 1, infusion tube 2, infusion pump 3, infusion tube 4, six-way valve 5, infusion tube 6, separating element 7 (chromatographic column), infusion tube 8 , detector 9, infusion tube 10, collector 11 and sample bottle 12, the main feature is to increase three three-way valves 21, 22, 23, a plunger pump 24, an electric control device, and collector 11 is both Sampling and collecting in one sample collector 11. The invention patent application can automatically complete the five processes of quantitative sampling, cleaning, sample separation, collection and discarding of samples, which overcomes the cumbersome manual operations in the prior art. However, because it includes three three-way valves 21, 22, and 23 respectively connected to the six-way valve 5 through pipelines, the manufacturing cost of the instrument is relatively high, the structure is relatively complicated, and maintenance is also difficult.

发明内容Contents of the invention

针对上述问题,本发明的目的是提供一种通过结构简单,成本较低,可实现自动流路控制分离的自动分离流路装置。In view of the above problems, the purpose of the present invention is to provide an automatic separation flow channel device which can realize automatic flow control separation with simple structure and low cost.

为实现上述,本发明采取以下技术方案:一种自动分离流路装置,它包括依次通过管路相互连接的一溶剂瓶、一输液泵、一六通阀、一分离元件、一收集器,一样品瓶、一柱塞泵和一废液瓶,其特征在于:它包括两个三通阀;第一个所述三通阀的三个端口分别通过管路连接所述溶剂瓶、六通阀和柱塞泵;第二个所述三通阀的三个端口分别通过管路连接所述收集器、分离元件和废液瓶;所述六通阀通过一管路直接连接所述收集器。In order to achieve the above, the present invention adopts the following technical solutions: an automatic separation flow path device, which includes a solvent bottle, an infusion pump, a six-way valve, a separation element, and a collector connected to each other through pipelines in sequence. A sample bottle, a plunger pump and a waste liquid bottle are characterized in that: it includes two three-way valves; the three ports of the first three-way valve are respectively connected to the solvent bottle and the six-way valve through pipelines and a plunger pump; the three ports of the second three-way valve are respectively connected to the collector, the separation element and the waste liquid bottle through pipelines; the six-way valve is directly connected to the collector through a pipeline.

在所述分离元件与第二个所述三通阀之间的管路上连接一检测器。A detector is connected on the pipeline between the separation element and the second three-way valve.

本发明由于采取以上技术方案,其具有以下优点:1、本发明由于在分离流路装置中,设置了两个三通阀、一个柱塞泵和驱动电路控制的电机,因此可以克服现有技术中繁琐的手工操作。2、本发明由于仅设置了两个三通阀,因此与专利号为200510114554.5的分离流路装置相比,结构简单,成本降低,通过控制两个三通阀与一个六通阀的切换,对柱塞泵和采样收集器进行控制,同样自动完成了样品的定量取样、清洗、样品分离、收集、丢弃五个过程。本发明结构简单,提高了分析效率和分析结果重复精度,降低了仪器生产成本和日常维护难度。Because the present invention adopts the above technical scheme, it has the following advantages: 1. The present invention can overcome the prior art due to two three-way valves, a plunger pump and a motor controlled by a drive circuit in the separation flow device. tedious manual operation. 2. Since only two three-way valves are provided in the present invention, compared with the separation flow device with the patent No. 200510114554.5, the structure is simple and the cost is reduced. By controlling the switching between two three-way valves and one six-way valve, the The plunger pump and sampling collector are controlled, and the five processes of quantitative sampling, cleaning, sample separation, collection and discarding of samples are also automatically completed. The invention has a simple structure, improves the analysis efficiency and the repeatability of the analysis results, and reduces the production cost of the instrument and the difficulty of daily maintenance.

附图说明Description of drawings

图1是普通手工操作的分离流路装置示意图Figure 1 is a schematic diagram of a separation flow path device operated manually

图2是专利申请号为200510114554.5的分离流路装置示意图Figure 2 is a schematic diagram of a separation flow device with patent application number 200510114554.5

图3是本发明分离流路装置示意图Fig. 3 is a schematic diagram of the separation flow path device of the present invention

图4是本发明的控制电路框图Fig. 4 is a control circuit block diagram of the present invention

图5是本发明另一分离流路装置示意图Fig. 5 is a schematic diagram of another separation channel device of the present invention

具体实施方式Detailed ways

下面结合附图和实施例,对本发明进行详细地描述。The present invention will be described in detail below in conjunction with the accompanying drawings and embodiments.

如图3所示,本发明是在现有手工操作流路的基础上进行的改进,本发明除了包括已有技术中的溶剂瓶1、管路2、输液泵3、管路4、六通阀5、管路6、分离元件7、管路8、检测器9、管路10、收集器11、样品瓶12以外,主要特征是增加了两个三通阀13、14和一个柱塞泵15,同时收集器11是兼具采样和收集于一身的收集器11。其中,第一个三通阀13的三个端口分别通过管路16连接溶剂瓶1、通过管路17连接六通阀5和通过管路18连接柱塞泵15;第二个三通阀14的三个端口分别通过管路10连接检测器9,通过管路19连接采样收集器11,通过管路20连接废液瓶,同时将六通阀5通过管路21连接收集器11。As shown in Figure 3, the present invention is an improvement on the basis of the existing manual operation flow path. In addition to including the solvent bottle 1, the pipeline 2, the infusion pump 3, the pipeline 4, and the six-way In addition to valve 5, pipeline 6, separation element 7, pipeline 8, detector 9, pipeline 10, collector 11, and sample bottle 12, the main features are that two three-way valves 13, 14 and a plunger pump are added 15. At the same time, the collector 11 is a collector 11 that combines sampling and collection. Wherein, the three ports of the first three-way valve 13 are respectively connected to the solvent bottle 1 by the pipeline 16, connected to the six-way valve 5 by the pipeline 17 and connected to the plunger pump 15 by the pipeline 18; the second three-way valve 14 The three ports are respectively connected to the detector 9 through the pipeline 10, connected to the sampling collector 11 through the pipeline 19, connected to the waste liquid bottle through the pipeline 20, and connected the six-way valve 5 to the collector 11 through the pipeline 21.

上述实施例中,分离元件7是可将液体混合样品分离的色谱柱,也可以是可将液体混合样品分离的凝胶柱,离子交换柱,逆流分离法所用的柱管,离心分配色谱法所用的分配槽,毛细管电泳分离样品所用的毛细管和溶剂精馏柱中的一种。In the above-mentioned embodiment, the separation element 7 is a chromatographic column that can separate the liquid mixed sample, and can also be a gel column that can separate the liquid mixed sample, an ion exchange column, a column tube used in countercurrent separation, and a centrifugal partition chromatography. One of the distribution tanks, capillary tubes and solvent distillation columns used for capillary electrophoresis separation of samples.

上述实施例中,分离元件7是可溶于溶剂的混合样品分离的色谱柱,也可以是可溶于溶剂的混合样品分离的凝胶柱,离子交换柱,逆流分离法所用的柱管,离心分配色谱法所用的分配槽,毛细管电泳分离样品所用的毛细管和溶剂精馏柱中的一种。In the foregoing embodiment, the separation element 7 is a chromatographic column for the separation of a solvent-soluble mixed sample, and may also be a gel column for the separation of a solvent-soluble mixed sample, an ion exchange column, a column tube for countercurrent separation, and a centrifuge. One of the distribution tanks used in partition chromatography, capillary tubes and solvent distillation columns used in capillary electrophoresis to separate samples.

如图3、图4所示,上述实施例中,各三通阀13、14、六通阀5、柱塞泵15均可以通过驱动电路控制各电机M1、M2、M3、M4驱动,比如电机M1带动三通阀13与溶剂瓶1相连、柱塞泵15与六通阀5相连,在进样和清洗进样针时完成对样品定量抽取和溶剂流向的控制;电机M2带动三通阀14控制进样和分离收集时的溶剂与样品流向;电机M3带动六通阀5控制将外部样品转移入分析流路的组件;电机M4带动柱塞泵15与三通阀13、14的配合,完成定量抽取溶剂和样品的功能。溶剂瓶1贮存并提供溶剂作为系统流动相,输液泵3入口通过管路2与溶剂瓶1连接,输液泵3可始终开启,抽取溶剂并供给整个管路流量恒定的流动溶剂。分离元件7是分离样品的组件;检测器9是检测样品的组件。本发明兼具采样和收集于一身的收集器11,既可以与样品瓶12组成采样组件,又可以与收集瓶(图中未示出)一起组成收集组件,收集瓶收集的是分离后的样品组分。As shown in Fig. 3 and Fig. 4, in the above-mentioned embodiment, each three-way valve 13, 14, six-way valve 5, and plunger pump 15 can be driven by controlling each motor M1, M2, M3, M4 through a drive circuit, such as a motor M1 drives the three-way valve 13 to connect with the solvent bottle 1, and the plunger pump 15 is connected to the six-way valve 5 to complete the quantitative extraction of the sample and the control of the solvent flow during sample injection and cleaning of the injection needle; the motor M2 drives the three-way valve 14 Control the solvent and sample flow during sample injection and separation and collection; the motor M3 drives the six-way valve 5 to control the components that transfer the external sample into the analysis flow path; the motor M4 drives the plunger pump 15 to cooperate with the three-way valves 13 and 14 to complete Quantitative extraction of solvents and samples. The solvent bottle 1 stores and provides the solvent as the mobile phase of the system. The inlet of the infusion pump 3 is connected to the solvent bottle 1 through the pipeline 2. The infusion pump 3 can always be turned on to extract the solvent and supply the flowing solvent with a constant flow rate throughout the pipeline. The separation element 7 is a component for separating samples; the detector 9 is a component for detecting samples. The collector 11 of the present invention combines sampling and collection, can form a sampling assembly with the sample bottle 12, and can form a collection assembly together with a collection bottle (not shown in the figure), and the collection bottle collects the separated sample components.

上述实施例中,根据样品进样、洗脱分析和需检测样品收集的要求,可以通过一般逻辑控制和驱动电路按照流路运行的顺序,启动不同的电机实现,并非本发明的特点,在此不再赘述。In the above-mentioned embodiment, according to the requirements of sample injection, elution analysis and collection of samples to be tested, it can be realized by starting different motors according to the sequence of flow path operation through general logic control and drive circuit, which is not a feature of the present invention. Herein No longer.

本发明需完成的动态过程包括:系统清洗、抽取样品、样品分离、收集和丢弃五个动态过程(如图3所示):The dynamic process that the present invention needs to complete comprises: five dynamic processes (as shown in Figure 3) of system cleaning, sample extraction, sample separation, collection and discarding:

1、自动分离流路装置处于初始状态时,溶剂流路方向为:溶剂瓶1-管路2-输液泵3-管路4-六通阀5-管路6-分离元件7-管路8-检测器9-管路10-三通阀14-管路20-废液瓶,此为样品分析管路清洗状态。1. When the automatic separation flow path device is in the initial state, the direction of the solvent flow path is: solvent bottle 1-line 2-infusion pump 3-line 4-six-way valve 5-line 6-separation element 7-line 8 -Detector 9-pipeline 10-three-way valve 14-pipeline 20-waste liquid bottle, this is the cleaning state of the sample analysis pipeline.

2、自动分离流路装置处于抽取样品状态时,采样收集器11插入样品瓶12中,电机M1带动三通阀13,使管路17与管路18连通,电机M2带动三通阀14使管路10与20连通,并封闭管路19,电机M3带动六通阀5中的换向杆连通管路17、21,电机M4带动柱塞泵15作抽拉动作,溶剂流路方向为:样品瓶12-采样收集器11-管路21-六通阀5-管路17-三通阀13-管路18-柱塞泵15,经过柱塞泵15的一次抽拉,便可以通过六通阀5中换向杆的切换达到自动定量采样的目的。2. When the automatic separation flow path device is in the state of extracting samples, the sampling collector 11 is inserted into the sample bottle 12, the motor M1 drives the three-way valve 13 to make the pipeline 17 communicate with the pipeline 18, and the motor M2 drives the three-way valve 14 to make the tube Lines 10 and 20 are connected, and the pipeline 19 is closed. The motor M3 drives the reversing rod in the six-way valve 5 to connect the pipelines 17 and 21. The motor M4 drives the plunger pump 15 to perform pulling action. The direction of the solvent flow path is: sample Bottle 12-sampling collector 11-pipeline 21-six-way valve 5-pipeline 17-three-way valve 13-pipeline 18-plunger pump 15, after one pull of the plunger pump 15, it can pass through the six-way The switching of the reversing lever in the valve 5 achieves the purpose of automatic quantitative sampling.

3、自动分离流路装置处于洗采样管路状态时,采样收集器11移出样品瓶12,三通阀14不动,电机M3带动六通阀5换向使其内的换向杆连通管路4、6,准备进行样品分离,电机M1带动三通阀13切换使管路16与18连通,电机M4带动柱塞泵15作抽拉动作,溶剂流路方向为:溶剂瓶1-管路16-三通阀13-管路18-柱塞泵15,电机M1带动三通阀13切换使管路17与18连通,电机M4带动柱塞泵15作推送动作,溶剂流路方向为:柱塞泵15-管路18-三通阀13-管路17-六通阀5-管路21-采样收集器11,将洗采样管路的废液排入废液池,柱塞泵15可以反复抽拉多次,以使采样管路清洗干净。3. When the automatic separation flow device is in the state of washing the sampling pipeline, the sampling collector 11 moves out of the sample bottle 12, the three-way valve 14 does not move, and the motor M3 drives the six-way valve 5 to change direction so that the reversing rod inside is connected to the pipeline 4, 6, ready for sample separation, the motor M1 drives the three-way valve 13 to switch to connect the pipeline 16 and 18, the motor M4 drives the plunger pump 15 to perform the pulling action, and the solvent flow direction is: solvent bottle 1-pipeline 16 -Three-way valve 13-Pipeline 18-Plunger pump 15, the motor M1 drives the three-way valve 13 to switch to connect the pipelines 17 and 18, and the motor M4 drives the plunger pump 15 to perform push action, the direction of the solvent flow path is: plunger Pump 15-pipeline 18-three-way valve 13-pipeline 17-six-way valve 5-pipeline 21-sampling collector 11, discharge the waste liquid from the washing sampling pipeline into the waste liquid pool, and the plunger pump 15 can repeatedly Pull several times to clean the sampling line.

4、自动分离流路装置处于样品分离状态时,溶剂流路方向为:溶液瓶1-管路2-输液泵3-管路4-六通阀5-管路6-分离元件7-管路8-检测器9-管路10-三通阀14-管路21-废液瓶。在洗脱过程中观察检测器9,将不需要的组分引入废液池,此为丢弃;一旦发现需要的组分出现峰值,电机M2带动三通阀14切换使管路10与19连通,便开始用收集瓶收集被检测到的样品组分。4. When the automatic separation flow path device is in the sample separation state, the direction of the solvent flow path is: solution bottle 1-line 2-infusion pump 3-line 4-six-way valve 5-line 6-separation element 7-line 8-detector 9-line 10-three-way valve 14-line 21-waste bottle. Observe the detector 9 during the elution process, and introduce unnecessary components into the waste liquid pool, which is discarded; once the peak value of the required components is found, the motor M2 drives the three-way valve 14 to switch to connect the pipelines 10 and 19, Then start to collect the detected sample components with the collection bottle.

5、第一个分离样品收集完成后,又回到初始状态,进行样品分析管路清洗。然后对余下的样品逐个重复前述分离过程,直到全部样品分离完毕为止。5. After the first separated sample is collected, return to the initial state and clean the sample analysis pipeline. Then repeat the aforementioned separation process one by one for the remaining samples until all the samples are separated.

如图5所示,本发明还提供了一种在确定了分离时间的条件下使用的分离流路装置,其与上述实施例相比,基本流路相同,不同之处在于:本实施例中的流路装置不包括检测器9,其中分离元件7通过管路8直接连接三通阀14。As shown in Figure 5, the present invention also provides a separation flow path device used under the condition that the separation time is determined. Compared with the above embodiment, the basic flow path is the same, the difference is that in this embodiment The flow path device does not include the detector 9, wherein the separation element 7 is directly connected to the three-way valve 14 through the pipeline 8.

Claims (2)

1.一种自动分离流路装置,它包括一溶剂瓶、一输液泵、一六通阀、一分离元件、一收集器、一样品瓶、一柱塞泵和一废液瓶,所述溶剂瓶通过管线依次连接所述输液泵、六通阀和分离元件的进口,其特征在于:它还包括两个三通阀;第一个所述三通阀的三个端口分别通过管路连接所述溶剂瓶、六通阀和柱塞泵;第二个所述三通阀的三个端口分别通过管路连接所述收集器的进口、分离元件的出口和废液瓶;所述六通阀通过一管路直接连接所述收集器,所述收集器兼具采样和收集于一身。1. An automatic separation flow path device, which comprises a solvent bottle, an infusion pump, a six-way valve, a separation element, a collector, a sample bottle, a plunger pump and a waste liquid bottle, the solvent The bottle is sequentially connected to the infusion pump, the six-way valve and the inlet of the separation element through pipelines, which is characterized in that it also includes two three-way valves; the three ports of the first three-way valve are respectively connected to the The solvent bottle, the six-way valve and the plunger pump; the three ports of the second three-way valve are respectively connected to the inlet of the collector, the outlet of the separation element and the waste liquid bottle through pipelines; the six-way valve The collector is directly connected through a pipeline, and the collector combines sampling and collection together. 2.如权利要求1所述的一种自动分离流路装置,其特征在于:在所述分离元件与第二个所述三通阀之间的管路上连接一检测器。2 . The automatic separation flow device according to claim 1 , wherein a detector is connected to the pipeline between the separation element and the second three-way valve. 3 .
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