WO2021249347A1 - 一种与液相色谱仪配套使用的静态进样和流分收集装置 - Google Patents

一种与液相色谱仪配套使用的静态进样和流分收集装置 Download PDF

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WO2021249347A1
WO2021249347A1 PCT/CN2021/098644 CN2021098644W WO2021249347A1 WO 2021249347 A1 WO2021249347 A1 WO 2021249347A1 CN 2021098644 W CN2021098644 W CN 2021098644W WO 2021249347 A1 WO2021249347 A1 WO 2021249347A1
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switching valve
sampling
electric
fraction
channel switching
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PCT/CN2021/098644
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English (en)
French (fr)
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赵维民
田海波
洪川
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上海贝高医疗科技有限公司
中国科学院上海药物研究所
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Publication of WO2021249347A1 publication Critical patent/WO2021249347A1/zh

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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
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • 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
    • G01N30/24—Automatic injection systems
    • 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
    • G01N30/80—Fraction collectors
    • G01N30/82—Automatic means therefor

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  • the utility model relates to the field of separation and purification of chemical and biological samples, in particular to a static sampling and flow collection device matched with a liquid chromatograph.
  • Liquid chromatography is based on the difference in the affinities of the components in the mixture to the two phases to achieve sample separation.
  • high-efficiency (also known as high-pressure) liquid chromatography using finer stationary phase supports and higher mobile phase pressures has been widely used by scientific research and production units, and has become an effective means of separation and purification of chemical and biological samples.
  • a complete set of high performance liquid chromatography equipment is generally composed of a high-pressure infusion pump, a chromatographic column, a gradient mixer, a column thermostat, an online degasser, a detector (ultraviolet/differential/evaporative light scattering/fluorescence, etc.), automatic or manual It is composed of sampler, fraction collector and corresponding analysis and control software.
  • the autosampler and fraction collector can reduce the repetitive operation and long-term duty of experiment and production personnel, improve work efficiency, and reduce labor costs.
  • the commercially available autosamplers all use mechanical motion arms and use X/Y/Z three-direction displacement for sample injection. They have strict restrictions on the position of the test tube/vial bottle. If the position is deviated, the sample cannot be injected normally. .
  • fraction collectors use a mechanical motion arm, which uses X/Y displacement for fraction collection, which has strict restrictions on the position of the test tube/vial bottle. If the position is deviated, the fraction cannot be collected normally.
  • the purpose of the present utility model is to provide a static sampling and fraction collection device used in conjunction with a liquid chromatograph. Its automatic sampling and fraction collection functions are achieved through the use of a syringe pump and an electric six-channel
  • the sampling valve, the electric multi-channel distribution valve and the corresponding control software are realized; it can realize the selective automatic sampling of the samples in different sample containers according to the needs, and the selective automatic sampling of the separated fractions according to the needs Collection: Because the instrument does not use the movement components in the traditional design, it can improve the reliability of long-term operation, and there is no limit to the amount of samples to be separated, which can realize the separation of a large number of samples for a long time and unattended.
  • a static sampling and fraction collection device used in conjunction with a liquid chromatograph including a programmable controller, an automatic sampler, and a fraction collector.
  • the automatic sampler includes a syringe pump and a first electric multi-channel switching valve And the electric six-channel injection valve; the outlet of the first electric multi-channel switching valve is connected to the electric six-channel injection valve through the main line, and the other five ports of the electric six-channel injection valve are respectively connected with the injection pump and occupying 2 ports.
  • the mobile phase of the quantitative loop and the liquid chromatography pump is connected to the inlet of the chromatographic column;
  • the fraction collector includes the programmable controller and the second electric multi-channel switching valve, the main line of the second electric multi-channel switching valve and the detection
  • the mobile phase of the second electric multi-channel switching valve is connected to the fraction collection container and the waste liquid collection container respectively;
  • the programmable controller includes a sample setting module and a D/A conversion module, and the sample setting
  • the fixed module is connected with the D/A conversion module, and the D/A conversion module is respectively connected with the first electric multi-channel switching valve, the electric six-channel injection valve and the syringe pump in the autosampler, and the second in the fraction collector Electric multi-channel switching valve connection.
  • the static sampling and fraction collection device used in conjunction with the liquid chromatograph of the present invention controls the channel switching of the first electric multi-channel switching valve through the sampling setting module and the D/A conversion module. Furthermore, it is possible to realize selective automatic sampling of samples in different sample containers without moving the mechanical arm according to needs.
  • the electric multi-channel switching valve adopts a multiple-in and one-out mode, and up to 24 sample injections.
  • the present invention can be further configured to further include a detector arranged outside for detecting the components of the flow component.
  • the inlet of the detector is connected with the outlet of the chromatographic column through a pipeline, and the outlet of the detector is connected to the second
  • the inlet of the electric multi-channel switching valve is connected by a pipeline.
  • the present invention can be further configured such that the programmable controller further includes an A/D conversion module, an information recognition module, and an information storage module.
  • the information recognition module is respectively connected to the A/D conversion module, the information storage module and the D
  • the /A conversion module is connected, and the detector is electrically connected with the A/D conversion module to transmit the detected stream component analog signal to the programmable controller.
  • the detector, A/D conversion module, information recognition module, information storage module and D/A conversion module can be used to control the switching of the channels of the second electric multi-channel switching valve, and then separate the flow points. Separate collection of the different components of the sample, which can accurately separate and collect the different components in the fraction, and the separation effect of the various components in the sample is better.
  • the present invention can be further configured to further include a touch screen, and the touch screen is connected to the programmable controller.
  • the present invention can be further configured such that the programmable controller further includes a wireless sending module and a wireless receiving module.
  • the remote control of the system and automatic software upgrade can be realized, and a single control software is used to integrate various control and analysis functions, which facilitates the control of various components.
  • the present invention can be further configured such that the sample injection system further includes a sample injection pipeline arrangement seat, which is arranged above the first electric multi-channel switching valve.
  • the pipelines connected to the first electric multi-channel switching valve are arranged to make them neat and orderly.
  • the flow collection system further includes a flow separation line arrangement seat, and the flow separation line arrangement seat is arranged above the second electric multi-channel switching valve.
  • the present invention can be further configured such that the programmable controller is also provided with a communication interface.
  • the system can be connected to external PC equipment.
  • the present invention can be further configured such that the touch screen and the programmable controller are integrated and arranged together.
  • Fig. 1 is a schematic diagram of a static sampling and fraction collection device used in conjunction with a liquid chromatograph according to an embodiment of the present invention.
  • FIG. 2 is a schematic structural view of the integrated sample processor in FIG. 1 from a perspective.
  • Fig. 3 is a schematic structural diagram of the integrated sample processor in Fig. 1 from another perspective.
  • Fig. 4 is a schematic diagram of the internal structure of the integrated sample processor in Fig. 2.
  • Fig. 5 is an internal system diagram of the programmable controller of the integrated sample processor in Fig. 1.
  • the utility model discloses a static sampling and fraction collection device used in conjunction with a liquid chromatograph, including an integrated sample processor, a chromatographic column 15, a liquid chromatographic pump 18, elution The liquid bottle 19 and the detector 17 for detecting the components of the fraction.
  • the integrated sample processor includes a programmable controller, a sampling system and a fraction collection system.
  • the sampling system includes a sample container 16, an injection pump 6, an electric three-way valve 5, an electric six-way injection valve 3, a first electric multi-channel switching valve 4, and an injection needle 7 connected to the injection pump 6, through the injection system The sample in the sample container 16 is sucked.
  • the capacity of the injection needle 7 can be selected by the user as required and set in the software of the touch screen 1, and its function is to suck samples in the sample container 16.
  • the function of the electric three-way valve 5 is to select sample injection or to eliminate waste liquid in the injection needle 7 according to needs.
  • the electric six-way injection valve 3 is also provided with a quantitative ring 14 for sucking and containing samples, and the electric six-way injection valve 3 can realize automatic cleaning of the pipeline and the injection needle.
  • the injection pump 6 is arranged in the casing 27 and includes a stepping motor 26, a screw 25, a switching power supply 22, a main control circuit board 23, and a stepping motor driver 24.
  • the fraction collection system includes a fraction collection container 20 and a waste liquid container.
  • the waste liquid container includes a cleaning waste liquid collection bottle 13 and a fraction waste liquid collection bottle 21.
  • the first electric multi-channel switching valve 4 includes 10 channels, the sample container 16 is provided with 10, and each sample container 16 is labeled, and each sample container 16 passes through each channel port of the first electric multi-channel switching valve 4 Each branch pipeline is connected.
  • the outlet of the first electric multi-channel switching valve 4 is connected to the inlet of the external chromatographic column 15 through the main line, and the injection pump 6 is arranged on the pipeline of the main line.
  • the first electric multi-channel switching valve of the autosampler part can be eliminated, and the sample connected to the electric six-channel switching valve can be used The sampling line directly sucks the sample solution to be separated.
  • the fraction collection system further includes a second electric multi-channel switching valve 9 which includes 10 channels.
  • a second electric multi-channel switching valve 9 which includes 10 channels.
  • the inlet of the second electric multi-channel switching valve 9 is connected to the outlet of the chromatographic column 15 through the main line, and the second electric multi-channel switching valve
  • Each channel of 9 is connected to the waste liquid container and each fraction collection container 20 through each branch line.
  • the sampling system also includes a sampling pipeline arrangement seat 2.
  • the sampling pipeline arrangement seat 2 is arranged above the first electric multi-channel switching valve 4, the sampling pipeline arrangement seat 2 is marked with a pipe number, and the sample pipeline arrangement seat 2 It is used to organize the branch pipelines connected to the first electric multi-channel switching valve 4 to make them neat and orderly.
  • the flow collection system also includes a flow separation pipeline arrangement seat 8.
  • the flow separation pipeline arrangement seat 8 is arranged above the second electric multi-channel switching valve 9, and the flow separation pipeline arrangement seat 8 is marked with a pipe number.
  • the flow separation pipeline arrangement seat 8 is used to organize the branch pipelines connected to the second electric multi-channel switching valve 9 to make it neat and orderly.
  • the backplane of the integrated sample processor is also provided with a power socket and a switch, on which a power switch and a fuse are integrated; the backplane is also provided with an electrical signal input terminal 10 connected to the detector 17 and a PC connected to it.
  • the inlet of the first electric multi-channel switching valve 4 is connected to each branch pipeline, and the sampling pipeline organizes the seat 2 and the sample
  • the container 16 is connected; the outlet of the first electric multi-channel switching valve 4 is connected to the inlet of the electric six-port injection valve 3 with a main line; the required quantitative loop 14 is connected to the ports 1 and 4 of the electric six-port injection valve 3 Connect the 6 ports of the electric six-way injection valve 3 with the inlet of the electric three-way valve 5; connect the outlet of the electric three-way valve 5 with the cleaning waste collection bottle 13; connect the injection needle 7 Install on the syringe pump 6, connect the inlet of the injection needle 7 to the bottom port of the electric three-way valve 5; connect the 2 ports of the electric six-way injection valve 3 to the external liquid chromatography pump 18 with a pipeline; The three ports of the six-port injection valve 3 are connected to the external chromatographic column 15 with pipelines; the outlet pipeline under
  • the sample When in use, the sample is injected through the injection needle 7 on the syringe pump 6. After the injection is completed, the eluent in the eluent bottle 19 is injected into the chromatographic column through the electric six-way injection valve 3 through the liquid chromatography pump 18 Inside, using the principle that the chromatographic column has different adsorption forces for different sample components, the sample components are separated, and then the fractions enter the detector 17 for component detection, and the detection information is fed back to the controller.
  • the static sampling and fraction collection device used in conjunction with the liquid chromatograph of the present invention also includes a touch screen 1, which has a built-in Android system or windows operating system, and the touch screen System control software is installed on the display 1.
  • the control software can control the sampling system, the first electric multi-channel switching valve 4, the electric six-port injection valve 3, and the second electric multi-channel switching valve 9. Draw the absorbance curve for the level signal. It can control the injection volume, injection speed, number of injections, injection interval, etc. of the injection system. By matching the injection time interval with the separation time of the chromatographic column 15, it can realize uninterrupted and repeated automatic injection. Can realize unattended, long-term sample separation.
  • the touch screen 1 is connected to a programmable controller, and the touch screen 1 is integrated with the programmable controller.
  • the programmable controller also includes an A/D conversion module, an information recognition module, and an information storage module.
  • the A/D conversion module is used to receive the analog signal fed back by the detector 17 and convert the analog signal into a digital signal.
  • the information identification module is respectively connected with the A/D conversion module, the information storage module and the D/A conversion module.
  • the D/A conversion module is respectively electrically connected with the first electric multi-channel switching valve 4, the second electric multi-channel switching valve 9 and the injection pump 6 to realize control.
  • the detector 17 is electrically connected to the A/D conversion module to transmit the detected stream component analog signal to the programmable controller.
  • the information recognition module is connected with the A/D conversion module to receive the converted digital signal and to identify whether the same signal has been stored in the information storage module. If there is, the storage information of the stored signal is queried through the information storage module, for example, which fraction collection container 20 is stored in, and a digital signal is sent to the D/A conversion module, and the D/A conversion module converts the digital signal into The analog signal is transmitted to the second electric multi-channel switching valve 9, and the second electric multi-channel switching valve 9 is controlled to collect the fraction in the fraction collection container 20 of the same fraction that has been collected before; if not, then the fraction is collected.
  • the component signal is transmitted to the information storage module for storage and records, and at the same time, a digital signal is sent to the D/A conversion module to control the second electric multi-channel switching valve 9 to collect the fraction into a new fraction collection container 20.
  • the programmable controller also includes an injection setting module.
  • the injection setting module is used to set single or multiple injection types, injection sequence, number of repetitive injections, injection time interval, and injection volume according to needs, and The fraction collection container 20 can be designated for each sample. By setting the sampling time interval reasonably, the separation capacity of the chromatographic column 15 can be fully and effectively utilized, the separation efficiency can be improved, and the effective separation of samples can be realized.
  • the sampling setting module is connected with the D/A conversion module to control the on and off of each channel of the first electric multi-channel switching valve 4 and the second electric multi-channel switching valve 9 to realize the set content.
  • the programmable controller also includes a wireless sending module and a wireless receiving module, which can realize the remote control and software upgrade of the system, and can monitor the operation of the equipment in real time.
  • the A/D conversion circuit can collect data from the signal of the detector 17 and display the separation curve of the flow component on the display screen.
  • the collection of the flow component can be controlled by the threshold method, the timing method and the peak shape method.
  • the threshold method is to set a threshold on the system software of the touch screen. Peaks higher than the threshold are all samples to be collected, and can be collected sequentially by controlling the second electric multi-channel switching valve 9.
  • the principle of the timing method is based on the high repeatability of the separation of the same sample on the chromatographic column 15. After the peak time of each peak shape is determined, the sample can be set in the software within a specific time period after each injection Collect, and can specify the collection container 20 for the collected fraction.
  • the peak shape method is based on the peak characteristics. It is collected according to the inflection point of the peak shape. Compared with the threshold method, the sample collection is more efficient. The two adjacent peaks can also be collected separately. This is something that the threshold method cannot do.
  • the static sampling and fraction collection device of the utility model used in conjunction with the liquid chromatograph firstly set the parameters in the system software program of the touch display screen 1 during use, including setting the type of sample and the sample injection Sequence, sample injection speed and sample volume, set sample interval time, set data collection time, set sample repetition times; set sample collection method, timing method, threshold method or peak-shaped peak method. After the setting is complete, click "Start" to carry out sample injection, separation and sample fraction collection.
  • the implementation principle of this embodiment is: the static sampling and fraction collection device used in conjunction with the liquid chromatograph of the present invention controls the first electric multi-channel switching valve 4 through the sampling setting module and the D/A conversion module Channel switching, and then optional automatic sampling of samples in different sample containers 16 according to needs; moreover, through the detector 17, A/D conversion module, information recognition module, information storage module and D/A conversion module, control The switching of the channels of the second electric multi-channel switching valve 9 automatically separates and collects the different components separated in the flow, which can accurately separate and collect the different components in the flow.
  • the static sampling and fraction collection device used in conjunction with the liquid chromatograph of the present invention can realize automatic and repeated sampling of multiple samples, and can realize fully automated sample separation operations, which greatly reduces labor costs and improves production efficiency. , And to ensure the consistency of the sample separation effect.
  • the instrument can realize remote equipment monitoring, remote data collection and online system upgrades.
  • the sampling system, fraction collection system, detector 17, touch screen 1 and wireless transceiver module are integrated into one, and the adaptability of each component is better, and a set of control system, a set of power supply, and a set of control system can be shared.
  • the control software and a chassis can greatly reduce the overall cost, and the after-sales and equipment maintenance are also greatly simplified, which is more convenient for users to operate and use, and has a higher cost-effective.

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Abstract

一种与液相色谱仪配套使用的静态进样和流分收集装置，包括可编程控制器、自动进样器和流分收集器，自动进样器包括注射泵(6)、第一电动多通道切换阀(4)和电动六通道进样阀(3)，流分收集器包括可编程控制器和第二电动多通道切换阀(9)，可编程控制器包括进样设定模块和D/A转换模块，进样设定模块与D/A转换模块连接。自动进样器可将进样管口固定置于样品容器底部，避免目前市售自动进样器常见的样品残留、样品损耗和机械故障等问题，通过结合采用电动多通道切换阀实现流分的收集，使液相色谱自动进样与流分收集功能集于一身，仪器构造简单、便于操作、占用空间小，可与各种型号的液相色谱仪配套使用。

Description

一种与液相色谱仪配套使用的静态进样和流分收集装置 技术领域
本实用新型涉及化学和生物样品的分离纯化领域，具体涉及一种与液相色谱仪配套使用的静态进样和流分收集装置。
背景技术
液相色谱法是基于混合物中各组分对两相亲和力的差别实现样品的分离。近年来，采用更细固定相担体和更高流动相压力的高效(又称高压)液相色谱法被科研和生产单位广泛应用，成为化学和生物样品分离纯化的有效手段。
一套完整的高效液相色谱装置一般是由高压输液泵、色谱柱、梯度混合器、柱温箱、在线脱气机、检测器(紫外/示差/蒸发光散射/荧光等)、自动或手动进样器、流分收集器及相应的分析控制软件等组成。其中的自动进样器和流分收集器可减少实验和生产人员的重复性操作和长时间值守，提高工作效率，降低人工成本。
目前市售的高效液相色谱仪有很多种品牌，都分别具有一定的用户群体。但现有的技术方案存在的缺陷是：
软件种类多，操作不方便，其中高压输液泵、自动进样器、检测器、流分收集器都有自己的控制/分析软件；
各种品牌的仪器分别由不同公司生产，互相兼容性差；
目前市售的自动进样器都是采用机械运动臂，采用X/Y/Z三个方向位移进行进样，其对试管/样品瓶位置有严格的限制，如位置出现偏差则无法正常进样。
目前市售的自动进样器通常采用金属进样针，无法插入样品瓶底将样品吸净，且在反复移动过程中可能产生样品的损耗。
流分收集器大多采用机械运动臂，采用X/Y两个方向位移进行流分收集，其对试管/样品瓶位置有严格的限制，如位置有偏差则无法正常收集流分。
自动进样器和流分收集器由于分别独立设计，采用运动组件多，仪器占用空间大，仪器功耗高、长时间运行的可靠性较差。
实用新型内容
针对现有技术的不足，本实用新型的目的是提供一种与液相色谱仪配套使用的静态进样和流分收集装置，其自动进样和流分收集功能通过采用注射泵、电动六通道进样阀、电动多通道分配阀和相应的控制软件来实现；可以实现根据需要对不同样品容器内的样品进行 选择性的自动进样，并根据需要，对分离后的流分进行选择性的收集；由于仪器中没有采用传统设计中的运动组件，可提高长时间运行的可靠性，并且对拟分离的样品量没有限制，可实现长时间、无人值守的大量样品的分离。
本实用新型的上述目的是通过以下技术方案得以实现的：
一种与液相色谱仪配套使用的静态进样和流分收集装置，包括可编程控制器、自动进样器和流分收集器，自动进样器包括注射泵、第一电动多通道切换阀和电动六通道进样阀；第一电动多通道切换阀的出口通过主管线与电动六通道进样阀相连，电动六通道进样阀的其余五个接口分别与注射泵、占用2个接口的定量环、液相色谱泵的流动相和色谱柱的入口相连；流分收集器包括所述可编程控制器和第二电动多通道切换阀组成,第二电动多通道切换阀的主管线与检测器的流动相相连，第二电动多通道切换阀的各分管线分别与流分收集容器和废液收集容器相连；可编程控制器包括进样设定模块和D/A转换模块，进样设定模块与D/A转换模块连接，D/A转换模块分别与自动进样器中的第一电动多通道切换阀、电动六通道进样阀和注射泵，以及流分收集器中的第二电动多通道切换阀连接。
通过采用上述技术方案，本实用新型的与液相色谱仪配套使用的静态进样和流分收集装置通过进样设定模块、D/A转换模块控制第一电动多通道切换阀的通道切换，进而可根据需要对不同样品容器内的样品在无需移动机械臂的情况下实现有选择的自动进样，该电动多通道切换阀采用多进一出方式，最多可达24路进样。
本实用新型在一较佳示例中可以进一步配置为，还包括设置于外界的用于检测流分成分的检测器，检测器的入口与色谱柱的出口通过管线相连，检测器的出口与第二电动多通道切换阀的入口通过管线相连。
通过采用上述技术方案，可以对经色谱柱分离后的流分进行成分检测。
本实用新型在一较佳示例中可以进一步配置为，可编程控制器还包括A/D转换模块、信息识别模块和信息存储模块，信息识别模块分别与A/D转换模块、信息存储模块和D/A转换模块连接，所述检测器与A/D转换模块电连接以将检测到的流分成分模拟信号传输至可编程控制器。
通过采用上述技术方案，可通过检测器、A/D转换模块、信息识别模块、信息存储模块和D/A转换模块，控制第二电动多通道切换阀的通道的切换，进而对流分中分离出的不同成分进行分开收集，能够精确的对流分中的不同成分进行分开收集，对样品中各种成分的分离效果更好。
本实用新型在一较佳示例中可以进一步配置为，还包括触控显示屏，触控显示屏与 所述可编程控制器连接。
本实用新型在一较佳示例中可以进一步配置为，所述可编程控制器还包括无线发送模块和无线接收模块。
通过采用上述技术方案，可实现该系统的远程控制和软件的自动升级，采用单一控制软件对各控制、分析功能进行集成，方便对各组件进行控制。
本实用新型在一较佳示例中可以进一步配置为，所述进样系统还包括进样管线整理座，进样管线整理座设置在第一电动多通道切换阀的上方。
通过采用上述技术方案，对第一电动多通道切换阀所连接的管线进行整理，使其整齐有序。
本实用新型在一较佳示例中可以进一步配置为，所述流分收集系统还包括流分管线整理座，流分管线整理座设置在第二电动多通道切换阀的上方。
本实用新型在一较佳示例中可以进一步配置为，所述可编程控制器上还设置有通讯接口。
通过采用上述技术方案，可将系统与外界PC设备相连。
本实用新型在一较佳示例中可以进一步配置为，所述触控显示屏与可编程控制器集成设置在一起。
通过采用上述技术方案，减小系统的尺寸大小，且增强其外观效果。
附图说明
图1是本实用新型实施例的与液相色谱仪配套使用的静态进样和流分收集装置的示意图。
图2是图1中的集成式样品处理器的一个视角的结构示意图。
图3是图1中的集成式样品处理器的另一个视角的结构示意图。
图4是图2中的集成式样品处理器的内部结构示意图。
图5是图1中的集成式样品处理器的可编程控制器的内部系统图。
图中，1、触控显示屏；2、进样管线整理座；3、电动六通进样阀；4、第一电动多通道切换阀；5、电动三通阀；6、注射泵；7、进样注射器；8、流分管线整理座；9、第二电动多通道切换阀；10、电信号输入端子；11、开关；12、RS232通讯接口；13、清洗废液收集瓶；14、定量环；15、色谱柱；16、样品容器；17、检测器；18、液相色谱泵；19、洗脱液瓶；20、流分收集容器；21、废液收集瓶；22、开关电源；23、主控电路板；24、步进电机驱动器；25、丝杆；26、步进电机；27、机壳。
具体实施方式
以下结合附图对本实用新型作进一步详细说明。
参照图1至图4，本实用新型公开了一种与液相色谱仪配套使用的静态进样和流分收集装置，包括集成式样品处理器、色谱柱15、液相色谱泵18、洗脱液瓶19和用于检测流分成分的检测器17。集成式样品处理器包括可编程控制器、进样系统和流分收集系统。进样系统包括样品容器16、注射泵6、电动三通阀5、电动六通进样阀3、第一电动多通道切换阀4以及与注射泵6相连的进样针7，通过进样系统对样品容器16内的样品进行吸取。进样针7的容量用户可根据需要选择，并在触控显示屏1软件中设定，其作用是在样品容器16中吸取样品。电动三通阀5的作用是根据需要选择进样或者排除进样针7中的废液。电动六通进样阀3上还设置有用于吸取容纳样品的定量环14，电动六通进样阀3可以实现对管路和进样针的自动清洗。注射泵6设置于机壳27内，包括步进电机26、丝杆25、开关电源22、主控电路板23、步进电机驱动器24。流分收集系统包括流分收集容器20和废液容器，废液容器包括清洗废液收集瓶13和流分废液收集瓶21。第一电动多通道切换阀4包括10个通道，样品容器16设置有10个，并对各样品容器16进行标号区分，各样品容器16分别与第一电动多通道切换阀4的各个通道口通过各分管线相连。第一电动多通道切换阀4的出口通过主管线与外界的色谱柱15的入口相连，注射泵6设置在主管线的管路上。在其他实施例中，当装置只用于重复进样单一样品时，作为一种简化装置，可取消自动进样器部分的第一电动多通道切换阀，用与电动六通道切换阀相连的样品进样管线直接吸取待分离样品溶液。
参照图1至图4，流分收集系统还包括第二电动多通道切换阀9，第二电动多通道切换阀9包括10个通道。流分收集容器20设置有9个，并对各流分收集容器20进行标号区分，第二电动多通道切换阀9的入口通过主管线与色谱柱15的出口相连，第二电动多通道切换阀9的各个通道与废液容器和各流分收集容器20通过各分管线相连。进样系统还包括进样管线整理座2，进样管线整理座2设置在第一电动多通道切换阀4的上方，进样管线整理座2上标记有管路编号，进样管线整理座2用于对第一电动多通道切换阀4所连接的分管线进行整理，使其整齐有序。流分收集系统还包括流分管线整理座8，流分管线整理座8设置在第二电动多通道切换阀9的上方，流分管线整理座8上标记有管路编号，流分管线整理座8用于对第二电动多通道切换阀9所连接的分管线进行整理，使其整齐有序。另外，集成式样品处理器的背板上还设置有电源插座和开关，其上集成了电源开关和保险丝；背板上还设置有和检测器17相连的电信号输入端子10、和PC相连的RS232通讯接口12、电源插座 和开关11。
本实用新型的与液相色谱仪配套使用的静态进样和流分收集装置在使用时，将第一电动多通道切换阀4的入口连接各支管线，并通过进样管线整理座2与样品容器16相连；将第一电动多通道切换阀4的出口用主管线与电动六通进样阀3的入口相连；将所需的定量环14与电动六通进样阀3的1口和4口相连，将电动六通进样阀3的6口用管线与电动三通阀5的入口相连；将电动三通阀5的出口用管线与清洗废液收集瓶13相连；将进样针7安装在注射泵6上，将进样针7的入口与电动三通阀5的底部端口相连；将电动六通进样阀3的2口用管线与外部的液相色谱泵18相连；将电动六通进样阀3的3口用管线与外部的色谱柱15相连；将外部的色谱柱15下方的出口用管线与外部的检测器17的入口相连；将外部的检测器17的出口用管线与第二电动多通道切换阀9的入口相连；将外部的检测器17的信号输出用电缆线与电信号输入端子10相连；将第二电动多通道切换阀9的出口用管线经流分管线整理座8连接到流分收集容器20里，将第二电动多通道切换阀9的最后一个出口用管线连接到一个大的流分废液收集瓶21中。使用时，通过注射泵6上的进样针7进行进样，进样完成之后通过液相色谱泵18将洗脱液瓶19内的洗脱液通过电动六通进样阀3注入到色谱柱内，利用色谱柱对不同样品成分的吸附力大小不同的原理，进行样品成分分离，然后流分进入到检测器17内进行成分检测，并将检测信息反馈给控制器。
参照图5，本实用新型的与液相色谱仪配套使用的静态进样和流分收集装置还包括触控显示屏1，触控显示屏1内置安卓系统或windows操作系统，并在该触控显示屏1上安装了系统控制软件。控制软件可对进样系统、第一电动多通道切换阀4、电动六通进样阀3、第二电动多通道切换阀9进行控制，还可通过电信号输入端子10将来自外部检测器17的电平信号绘制吸收度曲线。其可控制进样系统的进样量、进样速度、进样次数、进样间隔等，通过将进样时间间隔与色谱柱15分离时间相匹配，从而实现不间断的、反复自动进样，可以实现无人值守、长时间的样本分离。触控显示屏1与可编程控制器连接，且触控显示屏1与可编程控制器集成设置在一起。可编程控制器还包括A/D转换模块、信息识别模块和信息存储模块。A/D转换模块用于接收检测器17反馈的模拟信号，并将该模拟信号转换为数字信号。信息识别模块分别与A/D转换模块、信息存储模块和D/A转换模块连接。D/A转换模块分别与第一电动多通道切换阀4、第二电动多通道切换阀9和注射泵6电连接，以实现控制。检测器17与A/D转换模块电连接以将检测到的流分成分模拟信号传输至可编程控制器。信息识别模块与A/D转换模块连接，用于接收其转换的数字信号，并识别信息存储模块中是否已经存储过同样的信号。如果有，则通过信息存储模块查询已存储信号的存储信 息，例如，存储在哪个流分收集容器20中，并向D/A转换模块发出数字信号，D/A转换模块将该数字信号转换为模拟信号并传输至第二电动多通道切换阀9，控制第二电动多通道切换阀9将流分收集至之前已收集的相同流分的流分收集容器20中；如果没有，则将该流分成分信号传输至信息存储模块中存储记录，同时向D/A转换模块发出数字信号，控制第二电动多通道切换阀9将该流分收集至新的流分收集容器20中。可编程控制器还包括进样设定模块，进样设定模块用于根据需要设定单个或多个进样种类、进样顺序、重复进样次数、进样时间间隔和进样量，并可以为每种样品指定流分收集容器20。通过合理设定进样时间间隔可以充分有效的利用色谱柱15的分离能力，提高分离效率，实现样品的有效分离。进样设定模块与D/A转换模块连接，从而控制第一电动多通道切换阀4、第二电动多通道切换阀9各通道的通断，进而实现设定的内容。可编程控制器还包括无线发送模块和无线接收模块，可实现该系统的远程控制、软件升级，并能够实时监控设备的运行情况。
A/D转换电路可对检测器17信号进行数据采集，在显示屏上显示出流分成分的分离曲线，可通过阈值法、定时法和峰形法对流分成分采集进行控制。阈值法是通过在触控屏的系统软件上设置阈值，高于阈值的峰均属于待收集的样本，可通过控制第二电动多通道切换阀9依次进行收集。定时法的原理是根据色谱柱15对同一样本进行分离的高重复性进行的，在确定各个峰形的出峰时间后，可在软件上设定每次进样后的特定时间段内进行样品收集，并可指定收流分收集容器20。峰形法是根据出峰特征而定的，其根据判断峰形的拐点来收集的，相比阈值法，其样本收集更高效，对于相邻的两个峰也可进行分立的单独收集，而这是阈值法所无法做到的。
本实用新型的与液相色谱仪配套使用的静态进样和流分收集装置，在使用时先在触控显示屏1的系统软件程序中设置参数，包括设定进样的样品种类、进样次序、进样速度及进样量、设定进样间隔时间、设定数据采集时间、设定进样重复次数；设定样品采集方式，定时法、阈值法还是峰形分峰法。设置完成后点击“开始”进行样品的进样、分离及样品的流分收集。
本实施例的实施原理为：本实用新型的与液相色谱仪配套使用的静态进样和流分收集装置通过进样设定模块、D/A转换模块控制第一电动多通道切换阀4的通道切换，进而可根据需要对不同样品容器16内的样品可选择的自动进样；而且，通过检测器17、A/D转换模块、信息识别模块、信息存储模块和D/A转换模块，控制第二电动多通道切换阀9的通道的切换，进而对流分中分离出的不同成分自动进行分开收集，能够精确的对流分中的不同成分进行分开收集。另外，本实用新型的与液相色谱仪配套使用的静态进样和流分收集装置 可实现多样品的自动重复进样，可实现全自动化的样品分离操作，极大地降低人力成本、提高生产效率，并且保证了样品分离效果的一致性。此外，该仪器可实现远程设备监控，远程数据收集以及系统的在线升级。而且，将进样系统、流分收集系统、检测器17、触控显示屏1和无线收发模块集成于一体，各部件适配性更好，可以共用一套控制系统、一套电源、一套控制软件、一个机箱，因此可以大大降低总体成本，售后和设备维护上也大大简化，更便于用户操作和使用，具有更高的性价比。
本具体实施方式的实施例均为本实用新型的较佳实施例，并非依此限制本实用新型的保护范围，故：凡依本实用新型的结构、形状、原理所做的等效变化，均应涵盖于本实用新型的保护范围之内。

Claims (9)

  1. 一种与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：包括可编程控制器、自动进样器和流分收集器，自动进样器包括注射泵(6)、第一电动多通道切换阀(4)和电动六通道进样阀(3)；第一电动多通道切换阀(4)的出口通过主管线与电动六通道进样阀(3)相连，电动六通道进样阀(3)的其余五个接口分别与注射泵(6)、占用2个接口的定量环(14)、液相色谱泵的流动相和色谱柱(15)的入口相连；流分收集器包括所述可编程控制器和第二电动多通道切换阀(9)组成,第二电动多通道切换阀(9)的主管线与检测器(17)的流动相相连，第二电动多通道切换阀(9)的各分管线分别与流分收集容器(20)和废液收集容器相连；可编程控制器包括进样设定模块和D/A转换模块，进样设定模块与D/A转换模块连接，D/A转换模块分别与自动进样器中的第一电动多通道切换阀(4)、电动六通道进样阀(3)和注射泵(6)，以及流分收集器中的第二电动多通道切换阀(9)连接。
  2. 根据权利要求1所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：还包括设置于外界的用于检测流分成分的检测器(17)，检测器(17)的入口与色谱柱(15)的出口通过管线相连，检测器(17)的出口与第二电动多通道切换阀(9)的入口通过管线相连。
  3. 根据权利要求1或2所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：可编程控制器还包括A/D转换模块、信息识别模块和信息存储模块，信息识别模块分别与A/D转换模块、信息存储模块和D/A转换模块连接，所述检测器(17)与A/D转换模块电连接以将检测到的流分成分模拟信号传输至可编程控制器。
  4. 根据权利要求1或2所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：还包括触控显示屏(1)，触控显示屏(1)与所述可编程控制器连接。
  5. 根据权利要求1或2所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：所述可编程控制器还包括无线发送模块和无线接收模块。
  6. 根据权利要求1或2所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：所述自动进样器还包括进样管线整理座(2)，进样管线整理座(2)设置在第一电动多通道切换阀(4)的上方。
  7. 根据权利要求6所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：所述流分收集器还包括流分管线整理座(8)，流分管线整理座(8)设置在第二电动多通道切换阀(9)的上方。
  8. 根据权利要求1或2所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：所述可编程控制器上还设置有通讯接口。
  9. 根据权利要求4所述的与液相色谱仪配套使用的静态进样和流分收集装置，其特征在于：所述触控显示屏(1)与可编程控制器集成设置在一起。
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