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CN201799135U - Split nano-fiber solid phase extraction column - Google Patents

Split nano-fiber solid phase extraction column Download PDF

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CN201799135U
CN201799135U CN201020500026XU CN201020500026U CN201799135U CN 201799135 U CN201799135 U CN 201799135U CN 201020500026X U CN201020500026X U CN 201020500026XU CN 201020500026 U CN201020500026 U CN 201020500026U CN 201799135 U CN201799135 U CN 201799135U
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pipe
phase extraction
extraction column
tube
solid
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康学军
顾忠泽
曲子键
王羽
邓剑军
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NANJING DONGJIAN BIOLOGICAL TECHNOLOGY Co Ltd
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Southeast University
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Abstract

本实用新型公开了一种分体式纳米纤维固相萃取柱,包括样品存放管(1),其特征在于所述样品存放管(1)下端套接有纤维填装管(2),所述纤维填装管(2)内部充填纳米纤维作为柱填料。该萃取柱具有简化操作流程,提高富集效率,缩短操作时间等优点。相比于传统的固相萃取柱,吸附剂用量大大减少,制作和使用方便、快捷。

Figure 201020500026

The utility model discloses a split-type nanofiber solid-phase extraction column, which comprises a sample storage tube (1), and is characterized in that a fiber filling tube (2) is sleeved on the lower end of the sample storage tube (1), and the fiber filling tube (2) The inside of the filling tube (2) is filled with nanofibers as column packing. The extraction column has the advantages of simplifying the operation process, improving the enrichment efficiency, shortening the operation time and the like. Compared with traditional solid-phase extraction columns, the amount of adsorbent is greatly reduced, and it is convenient and fast to make and use.

Figure 201020500026

Description

分体式纳米纤维固相萃取柱 Split nanofiber solid phase extraction column

技术领域technical field

本发明属于微量或痕量物质纯化技术领域,具体涉及一种分体式纳米纤维固相萃取柱及其应用。The invention belongs to the technical field of purification of micro or trace substances, and in particular relates to a split nanofiber solid-phase extraction column and its application.

背景技术Background technique

现代分析技术向着快捷、微量、痕量、多组分、高选择性方向发展,各种新形精密仪器层出不穷,对样品前处理过程也提出了越来越高的要求。然而,分析操作时间的60%甚至更多是用在样品的前处理上,试验误差也大多来自样品前处理过程。固相萃取(Solid-Phase Extraction,简称SPE)是一种有效的微量或痕量物质分离净化手段,是近年发展起来一种样品预处理技术,由液固萃取和柱液相色谱技术相结合发展而来,主要用于样品的分离、纯化和浓缩,与传统的液液萃取法相比较可以提高分析物的回收率,更有效的将分析物与干扰组分分离,减少样品预处理过程,操作简单、省时、省力。广泛的应用在医药、食品、环境、商检、化工等领域。Modern analysis technology is developing towards fast, micro, trace, multi-component, and high selectivity. Various new types of precision instruments emerge in an endless stream, and higher and higher requirements are put forward for the sample pretreatment process. However, 60% or more of the analysis operation time is spent on sample pretreatment, and most of the experimental errors come from the sample pretreatment process. Solid-phase extraction (Solid-Phase Extraction, referred to as SPE) is an effective means of separation and purification of trace or trace substances. It is a sample pretreatment technology developed in recent years. It is developed by combining liquid-solid extraction and column liquid chromatography. It is mainly used for the separation, purification and concentration of samples. Compared with the traditional liquid-liquid extraction method, it can improve the recovery rate of analytes, more effectively separate analytes from interfering components, reduce the sample pretreatment process, and is easy to operate. ,save time and energy. Widely used in medicine, food, environment, commodity inspection, chemical industry and other fields.

SPE大多数用来处理液体样品,萃取、浓缩和净化其中的半挥发性和不挥发性化合物,也可用于固体样品,但必须先处理成液体。SPE装置由SPE小柱和辅件构成。SPE小柱由三部分组成,柱管、烧结垫和填料。SPE辅件一般有真空系统、真空泵、吹干装置、惰性气源、大容量采样器和缓冲瓶。目前的商品萃取柱大多数采用颗粒状填料(约在30~60μm),柱体材料多为塑料(通常为聚丙烯)、玻璃及不锈钢,两端均有多孔滤片、内装填料总重0.1~1g。使用柱形固相萃取装置时,一般经活化、样品的吸附萃取、洗脱等步骤将待测物洗脱并收集在最小体积(数毫升)的有机溶剂中,再用氮气吹脱浓缩至更小体积供分析。这些操作比较繁琐,富集效果不明显,而且操作时间长,影响试验效率。本发明为此而来。SPE is mostly used to process liquid samples to extract, concentrate and purify semi-volatile and non-volatile compounds. It can also be used for solid samples, but it must be processed into liquid first. The SPE device consists of SPE columns and accessories. SPE small column consists of three parts, column tube, sintered pad and packing. SPE accessories generally include vacuum system, vacuum pump, drying device, inert gas source, large-capacity sampler and buffer bottle. Most of the current commercial extraction columns use granular fillers (about 30-60 μm), and the column materials are mostly plastic (usually polypropylene), glass and stainless steel. 1g. When using a column solid-phase extraction device, the analyte is generally eluted and collected in a minimum volume (several milliliters) of organic solvent through steps such as activation, adsorption and extraction of the sample, and elution, and then blown off with nitrogen and concentrated to a higher concentration. Small volume for analysis. These operations are cumbersome, the enrichment effect is not obvious, and the operation time is long, which affects the test efficiency. The present invention comes to this end.

发明内容Contents of the invention

本发明目的在于提供一种分体式纳米纤维固相萃取柱,解决了现有技术中固相萃取操作比较繁琐、富集效果不明显、操作时间长等问题。The purpose of the present invention is to provide a split-type nanofiber solid-phase extraction column, which solves the problems in the prior art that the solid-phase extraction operation is cumbersome, the enrichment effect is not obvious, and the operation time is long.

为了解决现有技术中的这些问题,本发明提供的技术方案是:In order to solve these problems in the prior art, the technical solution provided by the invention is:

一种分体式纳米纤维固相萃取柱,包括样品存放管,其特征在于所述样品存放管下端套接有纤维填装管,所述纤维填装管内部充填纳米纤维作为柱填料。A split-type nanofiber solid-phase extraction column, including a sample storage tube, characterized in that the lower end of the sample storage tube is sleeved with a fiber filling tube, and the inside of the fiber filling tube is filled with nanofibers as a column filler.

优选的,所述样品存放管包括上、下端锥形管,所述上、下端锥形管通过锥形管较大端连接成一体。Preferably, the sample storage tube includes upper and lower tapered tubes, and the upper and lower tapered tubes are connected into one body through the larger end of the tapered tube.

优选的,所述纤维填装管包括充填纳米纤维的圆管,所述圆管管口为与下端锥形管管口套接配合的锥形管口。Preferably, the fiber-filled tube includes a circular tube filled with nanofibers, and the circular tube orifice is a tapered orifice that is socketed and fitted with the orifice of the tapered tube at the lower end.

优选的,所述圆管下端固定连接有集流管,所述集流管为锥形管,所述集流管与圆管连接处设置多孔隔板或多孔隔膜。Preferably, a collecting pipe is fixedly connected to the lower end of the round pipe, the collecting pipe is a tapered pipe, and a porous partition or a porous diaphragm is arranged at the connection between the collecting pipe and the round pipe.

优选的,所述样品存放管上端与加压装置密闭连接。Preferably, the upper end of the sample storage tube is airtightly connected with the pressurizing device.

优选的,所述加压装置选自注射器或气压泵。Preferably, the pressurizing device is selected from a syringe or an air pump.

本发明还提供了一种所述的分体式纳米纤维固相萃取柱在微量或痕量物质分离净化方面的应用。The present invention also provides an application of the split-type nanofiber solid-phase extraction column in the separation and purification of micro or trace substances.

本发明技术方案中纳米纤维固相萃取柱包括纤维填装管、样品存放管。纤维填装管、样品存放管两部分连接方式为套接(具体的,样品存放管下端套入纤维填装管内),纤维填装管内部填装纳米纤维,纤维填装管的主要部分为圆管,圆管上口为可套接样品存放管的锥形管口,圆管下端固定连接集流管。集流管可为锥形管,其管内具有一定的向下倾斜角度,如与竖直方向成5°的倾斜角,这样便于液体向下向集流管内集中流出,圆管与集流管连接处可设置多孔隔板或多孔隔膜,多孔隔板或多孔隔膜上设置有多个通孔,一方面方便样品通过,另一方面限制纳米纤维在圆管内。样品存放管包括上下锥形管,上锥形管为锥度较小的锥形管,便于使其与加压装置连接更为紧密。The nanofiber solid-phase extraction column in the technical solution of the present invention includes a fiber filling tube and a sample storage tube. The two parts of the fiber filling tube and the sample storage tube are connected by socket (specifically, the lower end of the sample storage tube is inserted into the fiber filling tube), the inside of the fiber filling tube is filled with nanofibers, and the main part of the fiber filling tube is a round The upper opening of the circular tube is a tapered nozzle that can be nested with the sample storage tube, and the lower end of the circular tube is fixedly connected to the collecting tube. The collecting pipe can be a tapered pipe, and the pipe has a certain downward inclination angle, such as an inclination angle of 5° with the vertical direction, so that it is convenient for the liquid to flow downward into the collecting pipe, and the round pipe is connected with the collecting pipe A porous partition or a porous diaphragm can be provided at the position, and a plurality of through holes are arranged on the porous partition or porous diaphragm, on the one hand, it is convenient for the sample to pass through, on the other hand, the nanofiber is restricted in the circular tube. The sample storage tube includes an upper and lower conical tube, and the upper conical tube is a conical tube with a smaller taper, which facilitates a tighter connection with the pressurizing device.

相对于现有技术中的方案,本发明的优点是:Compared with the scheme in the prior art, the advantages of the present invention are:

本发明技术方案得到了一种纳米纤维固相萃取柱,利用该纳米纤维固相萃取柱(为固体吸附剂)来富集、萃取样品,进行样品预处理,该萃取柱提供了简便的纳米纤维填装方式,且使用时更加方便,适合于批量化生产纳米纤维固相萃取柱。本发明还得到一种应用于医药生物复杂样品、环境样品、毒物及污染物的微量、痕量样品的快速富集、纯化前处理的器件和装置。The technical scheme of the present invention obtains a nanofiber solid-phase extraction column, which is used to enrich and extract samples and perform sample pretreatment by using the nanofiber solid-phase extraction column (which is a solid adsorbent). The filling method is more convenient to use, and it is suitable for mass production of nanofiber solid-phase extraction columns. The present invention also obtains a device and device for fast enrichment and pre-purification treatment of complex samples of medicine and biology, environmental samples, trace samples of poisons and pollutants.

本发明纳米纤维固相萃取柱方便纳米纤维填装,易于实现批量化生产,使基于纳米纤维的新型固相萃取柱生产与使用更加方便。本发明基于基于纳米纤维的固相萃取技术,在SPE的基础上充分发挥了纳米材料的高效吸附特性,吸、脱附快速、吸附剂用量大大减少,进而使用中可以减少脱附剂用量、省略挥发溶剂浓缩的步骤。以纳米纤维为吸附剂的固相萃取器件具有简化操作流程,提高富集效率,缩短操作时间等优点。相比于传统的固相萃取柱,由于吸附剂用量大大减少,所以对柱体需要新的设计,以满足新型固相萃取柱制作和使用方便、快捷的需要。The nanofiber solid-phase extraction column of the invention is convenient for nanofiber filling, and is easy to realize mass production, so that the production and use of the novel solid-phase extraction column based on nanofiber is more convenient. The present invention is based on the solid phase extraction technology based on nanofibers, and on the basis of SPE, the high-efficiency adsorption characteristics of nanomaterials are fully utilized, the absorption and desorption are fast, and the amount of adsorbent is greatly reduced, and the amount of desorbent can be reduced during use. A step in which the volatile solvent is concentrated. The solid-phase extraction device using nanofiber as the adsorbent has the advantages of simplifying the operation process, improving the enrichment efficiency, and shortening the operation time. Compared with the traditional solid phase extraction column, because the amount of adsorbent is greatly reduced, a new design of the column is required to meet the needs of making and using the new solid phase extraction column conveniently and quickly.

附图说明Description of drawings

下面结合附图及实施例对本发明作进一步描述:The present invention will be further described below in conjunction with accompanying drawing and embodiment:

图1为本发明实施例纳米纤维固相萃取柱的结构示意图;Fig. 1 is the structural representation of the nanofiber solid-phase extraction column of the embodiment of the present invention;

图2为本发明实施例纳米纤维固相萃取柱纤维填装管内部结构图;Fig. 2 is the internal structure diagram of the nanofiber solid phase extraction column fiber packing tube of the embodiment of the present invention;

图3为本发明实施例纳米纤维固相萃取柱使用手动操作方式连接示意图;Figure 3 is a schematic diagram of the connection of the nanofiber solid-phase extraction column in the embodiment of the present invention using manual operation;

图4为本发明实施例纳米纤维固相萃取柱使用气动操作方式连接示意图。Fig. 4 is a schematic diagram of connection of the nanofiber solid-phase extraction column in an embodiment of the present invention using a pneumatic operation method.

其中:1为样品存放管;2为纤维填装管;3为加压装置;11为上端锥形管;12为下端锥形管;21为圆管;22为集流管;23为多孔隔板,4为橡胶连接管。Among them: 1 is the sample storage tube; 2 is the fiber filling tube; 3 is the pressure device; 11 is the upper conical tube; 12 is the lower conical tube; 21 is the round tube; 22 is the collecting tube; 23 is the porous partition Plate, 4 is a rubber connecting pipe.

具体实施方式Detailed ways

以下结合具体实施例对上述方案做进一步说明。应理解,这些实施例是用于说明本发明而不限于限制本发明的范围。实施例中采用的实施条件可以根据具体厂家的条件做进一步调整,未注明的实施条件通常为常规实验中的条件。The above solution will be further described below in conjunction with specific embodiments. It should be understood that these examples are used to illustrate the present invention and not to limit the scope of the present invention. The implementation conditions used in the examples can be further adjusted according to the conditions of specific manufacturers, and the implementation conditions not indicated are usually the conditions in routine experiments.

实施例如图1~4所示,该分体式纳米纤维固相萃取柱,包括样品存放管1,所述样品存放管1下端套接有纤维填装管2,所述纤维填装管2内部充填纳米纤维作为柱填料。所述样品存放管1包括上、下端锥形管11、12,所述上、下端锥形管11、12通过锥形管较大端连接成一体。所述纤维填装管2包括充填纳米纤维的圆管21,所述圆管21管口为与下端锥形管管口套接配合的锥形管口。所述圆管21下端固定连接有集流管22,所述集流管22为锥形管,所述集流管22与圆管21连接处设置多孔隔板23或多孔隔膜。Embodiments shown in Figures 1 to 4, the split nanofiber solid phase extraction column includes a sample storage tube 1, the lower end of the sample storage tube 1 is sleeved with a fiber filling tube 2, and the inside of the fiber filling tube 2 is filled with Nanofibers are used as column packing. The sample storage tube 1 includes upper and lower tapered tubes 11, 12, and the upper and lower tapered tubes 11, 12 are connected into one body through the larger ends of the tapered tubes. The fiber filling tube 2 includes a circular tube 21 filled with nanofibers, and the nozzle of the circular tube 21 is a tapered nozzle that is socketed and fitted with the nozzle of the tapered tube at the lower end. The lower end of the round pipe 21 is fixedly connected with a collecting pipe 22 , the collecting pipe 22 is a tapered pipe, and the connection between the collecting pipe 22 and the round pipe 21 is provided with a porous partition 23 or a porous diaphragm.

使用时,所述样品存放管1上端与加压装置3密闭连接。根据使用方式的不同所述加压装置3选用注射器或气压泵。When in use, the upper end of the sample storage tube 1 is airtightly connected with the pressurizing device 3 . Said pressurizing device 3 selects a syringe or an air pump according to different ways of use.

装配时,首先将纳米纤维填装入纤维填装管内2,然后将样品存放管1插入纤维填装管2中,将所需试样注入样品存放管1,将橡胶连接管4与样品存放管1连接,最后将橡胶连接管4与注射器或气压泵3相连,即可使用。When assembling, first fill the nanofibers into the fiber filling tube 2, then insert the sample storage tube 1 into the fiber filling tube 2, inject the required sample into the sample storage tube 1, connect the rubber connecting tube 4 and the sample storage tube 1 connection, and finally connect the rubber connecting tube 4 with the syringe or the air pump 3, then it can be used.

如图3为手动操作方式,使用时,将样品注入样品存放管1中,然后通过橡胶连接管4与注射器3连接,推压注射器,可进行样品的分离纯化工作;如图4为气动操作方式,将样品注入样品存放管1中,然后通过橡胶连接管4与气动泵3连接,启动气动泵,为装置内增加气体压力,可进行样品的分离纯化。As shown in Figure 3, the manual operation mode is used. When in use, the sample is injected into the sample storage tube 1, and then connected to the syringe 3 through the rubber connecting tube 4, and the syringe is pushed to perform the separation and purification of the sample; as shown in Figure 4, the pneumatic operation mode , the sample is injected into the sample storage tube 1, and then connected to the pneumatic pump 3 through the rubber connecting tube 4, and the pneumatic pump is started to increase the gas pressure in the device, so that the separation and purification of the sample can be carried out.

上述实例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人是能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所做的等效变换或修饰,都应涵盖在本发明的保护范围之内。The above examples are only to illustrate the technical conception and characteristics of the present invention, and its purpose is to allow people familiar with this technology to understand the content of the present invention and implement it accordingly, and cannot limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention shall fall within the protection scope of the present invention.

Claims (6)

1. split type nanofiber solid-phase extraction column comprises that sample deposits pipe (1), it is characterized in that described sample deposits pipe (1) lower end and be socketed with fiber and load pipe (2), and described fiber is loaded pipe (2) inner filling nanofiber as column packing.
2. split type nanofiber solid-phase extraction column according to claim 1 is characterized in that described sample deposits pipe (1) and comprise upper and lower end conical pipe (11,12), and described upper and lower end conical pipe (11,12) links into an integrated entity by the bigger end of conical pipe.
3. split type nanofiber solid-phase extraction column according to claim 2 is characterized in that described fiber filling pipe (2) comprises the pipe (21) of filling nanofiber, and described pipe (21) mouth of pipe is the taper mouth of pipe that cooperates with lower end conical pipe mouth of pipe socket.
4. split type nanofiber solid-phase extraction column according to claim 3, it is characterized in that described pipe (21) lower end is fixedly connected with header (22), described header (22) is a conical pipe, and described header (22) is provided with porous barrier (23) or porous septum with pipe (21) junction.
5. split type nanofiber solid-phase extraction column according to claim 2 is characterized in that described sample deposits pipe (1) upper end and airtight connection of pressue device (3).
6. split type nanofiber solid-phase extraction column according to claim 5 is characterized in that described pressue device (3) is selected from syringe or pulsometer.
CN201020500026XU 2010-08-23 2010-08-23 Split nano-fiber solid phase extraction column Expired - Fee Related CN201799135U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101947393A (en) * 2010-08-23 2011-01-19 东南大学 Split-type nanometer fibre solid-phase extraction column and application thereof
CN102721587A (en) * 2012-06-26 2012-10-10 东南大学 Kit for analyzing and pre-treating sulfonamides in sample and pretreatment method
CN104020167A (en) * 2014-06-19 2014-09-03 天津医科大学 Method for detecting iodine in sample by utilizing polypyrrole nano fiber membrane
CN104771935A (en) * 2015-04-08 2015-07-15 北京普立泰科仪器有限公司 Solid-phase extraction device
CN118758708A (en) * 2024-09-09 2024-10-11 国科大杭州高等研究院 On-site enrichment instrument for new pollutants in water

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101947393A (en) * 2010-08-23 2011-01-19 东南大学 Split-type nanometer fibre solid-phase extraction column and application thereof
CN102721587A (en) * 2012-06-26 2012-10-10 东南大学 Kit for analyzing and pre-treating sulfonamides in sample and pretreatment method
CN104020167A (en) * 2014-06-19 2014-09-03 天津医科大学 Method for detecting iodine in sample by utilizing polypyrrole nano fiber membrane
CN104020167B (en) * 2014-06-19 2016-08-17 天津医科大学 A kind of use the method for iodine in polypyrrole nanofibers film detection sample
CN104771935A (en) * 2015-04-08 2015-07-15 北京普立泰科仪器有限公司 Solid-phase extraction device
CN104771935B (en) * 2015-04-08 2016-08-17 北京普立泰科仪器有限公司 A kind of solid-phase extraction device
CN118758708A (en) * 2024-09-09 2024-10-11 国科大杭州高等研究院 On-site enrichment instrument for new pollutants in water

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