CN107132299A - A kind of multichannel pack tomographic system - Google Patents
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Abstract
本发明公开了一种多通道聚束层析系统,所述系统由中央控制系统、提取物罐、洗脱溶剂罐、洗脱介质罐、压力泵、多通道聚束色谱柱系统、检测器和收集罐组成。其中,多通道聚束色谱柱系统由进料储存罐、十根色谱柱组成的聚束色谱柱和洗脱排出系统三个部分构成。本发明可以解决传统色谱分离技术中占地面积大、分离色谱柱之间存在压力差和时间差、生产较为粗放、缺乏智能化以及分离纯化的单体目标产物低的问题。提供一种多通道聚束层析系统装置,可用于多酚、黄酮、有机酸、多糖和多肽等多种生物活性物质的分离纯化。
The invention discloses a multi-channel bunching chromatography system, which consists of a central control system, an extract tank, an elution solvent tank, an elution medium tank, a pressure pump, a multi-channel bunching chromatography column system, a detector and Collection tank composition. Among them, the multi-channel bunching chromatographic column system consists of three parts: a feed storage tank, a bunching chromatographic column composed of ten chromatographic columns, and an elution discharge system. The invention can solve the problems of large occupied area, pressure difference and time difference between separation chromatographic columns, relatively extensive production, lack of intelligence and low monomer target product of separation and purification in the traditional chromatographic separation technology. A multi-channel beam chromatography system device is provided, which can be used for the separation and purification of various biologically active substances such as polyphenols, flavonoids, organic acids, polysaccharides and polypeptides.
Description
技术领域technical field
本发明涉及智能化色谱柱分离纯化的一种装置,属于化工领域。The invention relates to a device for separation and purification of an intelligent chromatographic column, which belongs to the field of chemical industry.
背景技术Background technique
目前色谱法及其相关应用技术几乎在所有领域均有应用,而色谱技术在科学研究和工业生产中具有举足轻重的作用,其具有分离精度高、设备简便、操作方便等特点。根据色谱分离技术的不同原理,其不仅可以被应用于物质成分的定量分析与检测,同时能够用于生物物质的制备分离和纯化,为工业化生产获得高纯度生物活性物质最重要、最有效的分离纯化技术。但是色谱分离技术在制备和工业规模上的发展还处于初步发展期,目前开发的各种色谱技术均具有一定的缺点和不足,传统色谱分离技术中占地面积大、分离色谱柱之间存在压力差和时间差、生产较为粗放、缺乏智能化。因而发展智能化、集约化、精确化、应用广等综合特性的连续操作色谱技术一直是人们所期望的。At present, chromatography and its related application technologies are used in almost all fields, and chromatography technology plays a pivotal role in scientific research and industrial production. It has the characteristics of high separation precision, simple equipment, and convenient operation. According to the different principles of chromatographic separation technology, it can not only be applied to the quantitative analysis and detection of material components, but also can be used for the preparation, separation and purification of biological substances, which is the most important and effective separation for industrial production to obtain high-purity biologically active substances Purification technology. However, the development of chromatographic separation technology on the preparation and industrial scale is still in the initial stage of development. Various chromatographic technologies developed at present have certain shortcomings and deficiencies. The traditional chromatographic separation technology occupies a large area and there is pressure between the separation chromatographic columns. Poor and time difference, relatively extensive production, lack of intelligence. Therefore, the development of continuous operation chromatographic technology with comprehensive characteristics such as intelligence, intensification, precision and wide application has always been expected by people.
此发明解决了传统色谱分离技术中占地面积大、分离色谱柱之间存在压力差和时间差、生产较为粗放、缺乏智能化以及分离纯化的单体目标产物低的问题。提供一种多通道聚束层析系统装置,可用于多酚、黄酮、有机酸、多糖和多肽等多种生物活性物质的分离纯化。This invention solves the problems of large footprint, pressure difference and time difference between separation columns, relatively extensive production, lack of intelligence, and low separation and purification of monomeric target products in traditional chromatographic separation technology. A multi-channel beam chromatography system device is provided, which can be used for the separation and purification of various biologically active substances such as polyphenols, flavonoids, organic acids, polysaccharides and polypeptides.
发明内容Contents of the invention
本发明的目的是为了解决传统色谱分离技术中占地面积大、分离色谱柱之间存在压力差和时间差、生产较为粗放、缺乏智能化以及分离纯化的单体目标产物低的问题。提供一种多通道聚束层析系统装置,可用于多酚、黄酮、有机酸、多糖和多肽等多种生物活性物质的分离纯化。本发明所述的多通道聚束层析系统装置,它包括中央控制系统、提取物罐、洗脱溶剂罐、洗脱介质罐、压力泵、多通道聚束色谱柱系统、检测器和收集罐;收集罐1、2和3的高度h4和直径d1均为1.13m。The purpose of the present invention is to solve the problems of large occupied area, pressure difference and time difference between separation chromatographic columns, relatively extensive production, lack of intelligence and low separation and purification of monomeric target products in traditional chromatographic separation technology. A multi-channel beam chromatography system device is provided, which can be used for the separation and purification of various biologically active substances such as polyphenols, flavonoids, organic acids, polysaccharides and polypeptides. The multi-channel bunching chromatography system device of the present invention comprises a central control system, an extract tank, an eluting solvent tank, an eluting medium tank, a pressure pump, a multi-channel bunching chromatography column system, a detector and a collecting tank ; The height h4 and diameter d1 of the collection tanks 1, 2 and 3 are all 1.13m.
多通道聚束色谱柱系统包括进料储存罐、十根色谱柱组成的聚束色谱柱和洗脱排出系统。进料储存罐的顶端有进水口、进料口和广口视窗,其底部有介质出口,进料储存罐内部与十根色谱柱联通。进料储存罐的高度h1为1.5 m;The multi-channel bunching column system includes a feed storage tank, a bunching column composed of ten columns and an elution discharge system. The top of the feed storage tank has a water inlet, a feed port and a wide opening window, and the bottom has a medium outlet, and the inside of the feed storage tank communicates with ten chromatographic columns. The height h1 of the feed storage tank is 1.5 m;
十根色谱柱的高度h2为3m,每根色谱柱的直径d2为30cm,每根色谱柱的底部安装有80目的衬板;The height h2 of the ten chromatographic columns is 3m, the diameter d2 of each chromatographic column is 30cm, and an 80-mesh liner is installed at the bottom of each chromatographic column;
多通道聚束色谱柱系统的洗脱排出口系统呈漏斗状,高度h3为15cm,十根色谱柱的出液口与其相通,洗脱排出口系统可以拆卸,洗脱排出口系统上具有反冲阀、废液排出阀和洗脱液排出阀;The elution outlet system of the multi-channel bunching chromatographic column system is funnel-shaped, and the height h3 is 15cm. The liquid outlets of the ten chromatographic columns are connected with it. The elution outlet system can be disassembled, and the elution outlet system has backflush valve, waste liquid discharge valve and eluent discharge valve;
提取物罐、洗脱溶剂罐和洗脱介质罐并列设置,提取物罐、洗脱溶剂罐和洗脱介质罐的上端口分别通过一个接收回流阀门与回流管的另一端口相连通;The extract tank, the elution solvent tank and the elution medium tank are arranged side by side, and the upper ports of the extract tank, the elution solvent tank and the elution medium tank are respectively connected to the other port of the return pipe through a receiving return valve;
提取物罐、洗脱溶剂罐和洗脱介质罐的下端口分别通过一个出料阀门和一个进料管的一个端口相连通,所述进料管上设置有压力泵。The lower ports of the extract tank, the elution solvent tank and the elution medium tank are respectively connected through a discharge valve and a port of a feed pipe, and a pressure pump is arranged on the feed pipe.
收集罐共有n个,n为自然数,且n= 3~10,每个收集罐的上端口分别洗脱排出口相连,并通过中央控制系统控制洗脱排出口到每个收集罐的开关;There are n collection tanks in total, n is a natural number, and n=3~10, the upper port of each collection tank is connected to the elution outlet respectively, and the switch of the elution outlet to each collection tank is controlled by the central control system;
收集罐的下端口分别通过一个出料阀门与溶剂回收系统相连,所述回收系统上设置有压力泵。The lower port of the collection tank is respectively connected with a solvent recovery system through a discharge valve, and a pressure pump is arranged on the recovery system.
基于上述多通道聚束色谱柱系统装置,其特征在于,该方法涉及以下步骤:Based on the above-mentioned multi-channel beam-forming chromatographic column system device, it is characterized in that the method involves the following steps:
步骤一,使得所述多通道聚束色谱柱系统内的十个色谱柱处于并联模式,将洗脱介质罐中的分离纯化介质通过压力泵转移到进料储存罐中,然后填充至每个色谱柱中;Step 1, make the ten chromatographic columns in the multi-channel bunching chromatographic column system in parallel mode, transfer the separation and purification medium in the elution medium tank to the feed storage tank through a pressure pump, and then fill it into each chromatographic column column;
步骤二,将提取物罐中的物料通过压力泵转移到进料储存罐中,然后上样到每个色谱柱中;Step 2, the material in the extract tank is transferred to the feed storage tank through a pressure pump, and then loaded into each chromatographic column;
步骤三,将洗脱溶剂罐中的洗脱溶剂通过压力泵转移到进料储存罐中,然后对每个色谱柱进行同时洗脱;Step 3, the elution solvent in the elution solvent tank is transferred to the feed storage tank through a pressure pump, and then each chromatographic column is eluted simultaneously;
步骤四,检测器通过对洗脱液进行分析检测,对洗脱得到的生物物质进行自动分类收集,相应得进入到收集罐1~n;Step 4, the detector automatically classifies and collects the eluted biological substances by analyzing and detecting the eluent, and correspondingly enters the collection tanks 1~n;
步骤五,洗脱结束后,打开洗脱排出口系统上的反冲阀和进料储存罐上的介质排出口,可以将所有色谱柱中的洗脱介质反冲出来。Step 5, after the elution is completed, open the backflush valve on the elution outlet system and the medium outlet on the feed storage tank to backflush the elution medium in all chromatographic columns.
本发明的优点:Advantages of the present invention:
1、可用于多酚、黄酮、有机酸、多糖和多肽等多种生物活性物质的分离纯化;1. It can be used for the separation and purification of various biologically active substances such as polyphenols, flavonoids, organic acids, polysaccharides and polypeptides;
2、能够保证多个色谱柱压力一致性和进料洗脱的同步化;2. It can ensure the pressure consistency of multiple chromatographic columns and the synchronization of feed elution;
3、一体化涉及,大大节省了空间和占地面积;3. Integrated design greatly saves space and floor space;
4、固相介质更换方便快捷;4. The replacement of solid phase medium is convenient and quick;
5、基本实现色谱分离纯化的智能化和自动化。5. Basically realize the intelligence and automation of chromatographic separation and purification.
附图说明Description of drawings
图1为本发明所述多通道聚束层析系统装置的结构示意图;Fig. 1 is a schematic structural view of the multi-channel beamforming chromatography system device of the present invention;
图2为本发明所述多通道聚束层析色谱柱的正面剖面图;Fig. 2 is the front sectional view of the multi-channel bunching chromatography column of the present invention;
图3为本发明所述多通道聚束层析系统中央控制系统示意图。Fig. 3 is a schematic diagram of the central control system of the multi-channel beamforming chromatography system of the present invention.
具体实施方式detailed description
下面结合附图对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。The technical solution of the present invention will be further described below in conjunction with the accompanying drawings, but it is not limited thereto. Any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention should be covered by the present invention. within the scope of protection.
实施例1Example 1
如图1所示,本发明提供的多通道聚束层析系统由1提取物储存罐、2洗脱溶剂储存罐、3洗脱介质储存罐、4压力泵、5中央控制系统、8多通道聚束色谱柱系统、9检测器、11收集罐3、12收集罐2和13收集罐1等部分组成;收集罐1、2和3的高度h4和直径d1均为1m ~ 4m。As shown in Figure 1, the multi-channel buncher chromatography system provided by the present invention consists of 1 extract storage tank, 2 elution solvent storage tanks, 3 elution medium storage tanks, 4 pressure pumps, 5 central control systems, 8 multi-channel It is composed of bunching column system, 9 detectors, 11 collection tank 3, 12 collection tank 2 and 13 collection tank 1; the height h4 and diameter d1 of collection tanks 1, 2 and 3 are all 1m ~ 4m.
如图1所示,多通道聚束色谱柱系统由6进料储存罐、7十根色谱柱组成的聚束色谱柱和10洗脱排出系统三个部分构成,如图2所示,整个多通道聚束色谱柱系统包括10个色谱柱,每个色谱柱里面填充的介质可以更换,2所指的为实心区域,10个色谱柱为一个整体从而形成一个圆柱体的多通道聚束色谱柱系统;每个色谱柱的相关参数:直径20 ~ 60 cm,长度:1m ~ 4m,容量8L ~ 20L;As shown in Figure 1, the multi-channel bunching chromatographic column system consists of three parts: 6 feed storage tanks, 7 dozen chromatographic columns, and 10 elution discharge systems. As shown in Figure 2, the entire multi-channel The channel bunching column system includes 10 chromatographic columns, the medium filled in each chromatographic column can be replaced, 2 refers to the solid area, and the 10 chromatographic columns are integrated to form a cylindrical multi-channel bunching chromatographic column System; the relevant parameters of each chromatographic column: diameter 20 ~ 60 cm, length: 1m ~ 4m, capacity 8L ~ 20L;
如图1所示F1、F2和F3分别为3洗脱介质储存罐、2洗脱溶剂储存罐和1提取物储存罐的阀门开关;F4为介质出口阀门开关;F5为反冲阀门开关;F6为洗脱废弃液排出阀门开关;F7为洗脱液排出阀门开关;F8为洗脱液排入收集罐1阀门开关;F9为洗脱液排入收集罐2阀门开关;F10为洗脱液排入收集罐3阀门开关;As shown in Figure 1, F1, F2 and F3 are respectively the valve switches of 3 elution medium storage tanks, 2 elution solvent storage tanks and 1 extract storage tank; F4 is the medium outlet valve switch; F5 is the recoil valve switch; F6 F7 is the eluent discharge valve switch; F8 is the eluent discharge into the collection tank 1 valve switch; F9 is the eluent discharge into the collection tank 2 valve switch; F10 is the eluent discharge Into the collection tank 3 valve switch;
如图1和3所示,所述多通道聚束色谱柱系统中央控制系统可以对阀门F1、F2、和F3进行控制,从而对整个分离过程进行操作;As shown in Figures 1 and 3, the central control system of the multi-channel bunching chromatographic column system can control valves F1, F2, and F3, thereby operating the entire separation process;
如图1和3所示,所述多通道聚束色谱柱系统中央控制系统通过检测器检测分析后,可以对阀门F8、F9和F10进行控制,从而实现对不同洗脱生物活性物质进行分类;As shown in Figures 1 and 3, the central control system of the multi-channel bunching chromatographic column system can control the valves F8, F9 and F10 after detection and analysis by the detector, so as to realize the classification of different eluting biologically active substances;
检测器装置运行时所需温度:18 ~ 26℃;The temperature required for the operation of the detector device: 18 ~ 26°C;
检测器装置运行时的压力为1MPa ~ 8MPa;The operating pressure of the detector device is 1MPa ~ 8MPa;
所述多通道聚束层析系统压力泵4同时用于提取物罐1、洗脱溶剂储存罐2和洗脱介质储存罐3中的物质进入系统,压力泵4的相关参数:流量为0.1 mL/min ~ 200 mL/min;工作电压为220V,50Hz;耗电量为1.5 kW ~3.0 kW。The pressure pump 4 of the multi-channel bunching chromatography system is simultaneously used for the substances in the extract tank 1, the elution solvent storage tank 2 and the elution medium storage tank 3 to enter the system, and the relevant parameters of the pressure pump 4: the flow rate is 0.1 mL /min ~ 200 mL/min; working voltage is 220V, 50Hz; power consumption is 1.5 kW ~3.0 kW.
实施例2Example 2
如图1所示,打开阀门F1,打开压力泵4,保证其他阀门关闭,使得所述多通道聚束色谱柱系统内的十个色谱柱处于并联模式,将洗脱介质罐3中的分离纯化介质通过压力泵转移到进料储存罐6中,然后进而通过重力作用填充至每个色谱柱中,保证介质在色谱柱中紧实;As shown in Figure 1, open the valve F1, open the pressure pump 4, and ensure that other valves are closed, so that the ten chromatographic columns in the multi-channel bunching chromatographic column system are in parallel mode, and the separation and purification in the elution medium tank 3 The medium is transferred to the feed storage tank 6 through a pressure pump, and then filled into each chromatographic column by gravity to ensure that the medium is compacted in the chromatographic column;
打开阀门F3,打开压力泵4,保证其他阀门关闭,将1提取物罐中的物料通过压力泵转移到进料储存罐中,然后上样到每个色谱柱中;Open the valve F3, turn on the pressure pump 4, ensure that other valves are closed, transfer the material in the 1 extract tank to the feed storage tank through the pressure pump, and then load the sample into each chromatographic column;
打开阀门F2和F7,打开压力泵4,保证其他阀门关闭,将洗脱溶剂罐中的洗脱溶剂通过压力泵转移到进料储存罐中,然后对每个色谱柱进行同时洗脱;检测器通过对洗脱液进行分析检测,对洗脱得到的生物物质进行自动分类收集,通过PLC中央控制系统控制阀门F8、F9和F10,使得相应的生物活性物质分别进入到收集罐1~n;Open valves F2 and F7, turn on pressure pump 4, ensure that other valves are closed, transfer the elution solvent in the elution solvent tank to the feed storage tank through the pressure pump, and then simultaneously elute each chromatographic column; Through the analysis and detection of the eluent, the eluted biological substances are automatically classified and collected, and the valves F8, F9 and F10 are controlled by the PLC central control system, so that the corresponding biologically active substances enter the collection tanks 1~n respectively;
洗脱结束后,打开洗脱排出口系统上的反冲阀F5和进料储存罐上的介质排出口F4,保证其他阀门关闭,通过向反冲阀F5注入相应得洗涤溶剂,可以将所有色谱柱中的洗脱介质反冲出来;并对整个色谱柱系统进行清洗。After the elution is completed, open the backflush valve F5 on the elution outlet system and the medium outlet F4 on the feed storage tank to ensure that other valves are closed. By injecting the corresponding washing solvent into the backflush valve F5, all chromatographic The elution medium in the column is backflushed; and the entire chromatographic column system is cleaned.
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| CN108495099A (en) * | 2018-06-05 | 2018-09-04 | 哈尔滨工业大学 | A kind of novel compositions annular arrangement chromatography video monitoring system |
| CN109954296A (en) * | 2018-12-12 | 2019-07-02 | 江苏哈工药机科技股份有限公司 | A kind of separation and purification device and separation and purification method of anthocyanin |
| CN110201420A (en) * | 2019-06-27 | 2019-09-06 | 上海渔霁生物技术有限公司 | A kind of chromatographic system and method separating organic acid and organic acid esters |
| CN113769438A (en) * | 2021-10-15 | 2021-12-10 | 温州大学 | A large-diameter chromatographic stationary phase with a double monolithic structure and its in-situ preparation method |
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| CN110201420B (en) * | 2019-06-27 | 2024-07-19 | 上海渔霁生物技术有限公司 | Chromatographic system and method for separating organic acid and organic acid ester |
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