阅读说明：本技术 一种高通量二噁英样品前处理净化装置 (High flux dioxin sample pretreatment purifier ) 是由 张维 程劼 王培龙 洪靖 张苏 于 2020-12-24 设计创作，主要内容包括：本发明公开了一种高通量二噁英样品前处理净化装置,包括净化柱,加液管,与加液管相连接的喷管,用于探测净化柱中液体液位的探测器,用于固定喷管和探测器的定位夹持装置,用于移动定位夹持装置使之实现X轴、Y轴和Z轴方向移动的传动运动组件；当所述传动运动组件动作使定位夹持装置位于玻璃柱架的上方时,所述定位夹持装置所夹持的喷管数量、位置排列与净化柱的数量、位置排列相一致,所述喷管向净化柱加液,所述探测器并依次循环探测净化柱中液体液位的高度变化。本发明的高通量二噁英样品前处理净化装置,可以同时向多达20个净化柱加入指定溶剂,并同步完成净化柱淋洗、移柱和收集提取液工作,实现二噁英样品高通量、全自动净化。(The invention discloses a high-flux dioxin sample pretreatment purifying device which comprises a purifying column, a liquid feeding pipe, a spray pipe connected with the liquid feeding pipe, a detector for detecting the liquid level in the purifying column, a positioning and clamping device for fixing the spray pipe and the detector, and a transmission motion assembly for moving the positioning and clamping device to realize the movement of the positioning and clamping device in the X-axis direction, the Y-axis direction and the Z-axis direction; when the transmission motion assembly acts to enable the positioning and clamping device to be located above the glass column frame, the number and the position arrangement of the spray pipes clamped by the positioning and clamping device are consistent with those of the purification columns, liquid is added to the purification columns through the spray pipes, and the detector sequentially and circularly detects the height change of the liquid level in the purification columns. The high-flux dioxin sample pretreatment purifying device can simultaneously add the specified solvent into up to 20 purifying columns, synchronously complete the operations of purifying column leaching, column moving and extracting solution collecting, and realize the high-flux full-automatic purification of the dioxin sample.)

1. The utility model provides a high flux dioxin sample pretreatment purifier which characterized in that: the device comprises a purifying column, a liquid feeding pipe, a spray pipe connected with the liquid feeding pipe, a detector for detecting the liquid level of liquid in the purifying column, a positioning and clamping device for fixing the spray pipe and the detector, and a transmission motion assembly for moving the positioning and clamping device to realize the movement in the X-axis direction, the Y-axis direction and the Z-axis direction; when the transmission motion assembly acts to enable the positioning and clamping device to be located above the glass column frame, the number and the position arrangement of the spray pipes clamped by the positioning and clamping device are consistent with those of the purification columns, liquid is added to the purification columns through the spray pipes, and the detector sequentially and circularly detects the height change of the liquid level in the purification columns.

2. The high-throughput dioxin sample pretreatment purification apparatus according to claim 1, characterized in that: the high-flux dioxin sample pretreatment purifying device also comprises a solution bottle for providing solution and a liquid adding pump for pumping the solution in the solution bottle, wherein the outlet of the liquid adding pump is connected with a liquid adding pipe; the number of the solution bottles and the liquid adding pumps is matched with that of the liquid adding pipes.

3. The high-throughput dioxin sample pretreatment purification apparatus according to claim 2, characterized in that: the transmission motion assembly comprises an X-axis lead screw, an X-axis slide block which is driven by the X-axis lead screw to slide along the X-axis direction is sleeved on the X-axis lead screw, a Z-axis lead screw which extends downwards is arranged on the X-axis slide block in a penetrating mode, a Z-axis slide block which is driven by the Z-axis lead screw to slide along the Z-axis direction is fixed on the Z-axis lead screw, a Y-axis lead screw which extends in a penetrating mode is arranged on the Z-axis slide block and in the horizontal direction, a Y-axis slide block which is driven by the Y-axis lead screw to slide along the Y-axis direction is sleeved on the Y-axis lead.

4. The high-throughput dioxin sample pretreatment purification apparatus according to claim 3, characterized in that: one end of the X-axis lead screw is provided with an X-axis motor, one end of the Z-axis lead screw is provided with a Z-axis motor, and one end of the Y-axis lead screw is provided with a Y-axis motor.

5. The high-throughput dioxin sample pretreatment purification apparatus according to claim 3, characterized in that: the positioning and clamping device is a fixed plate, and the fixed plate is provided with a plurality of insertion holes for insertion of the spray pipe and the detector; one of the jacks is used for inserting the detector, and the other jacks are used for inserting the spray pipe.

6. The high-throughput dioxin sample pretreatment purification apparatus according to claim 1, characterized in that: the high-flux dioxin sample pretreatment purifying device also comprises a glass column frame for inserting purifying columns, wherein the glass column frame comprises a lower bottom plate, an upper bottom plate and supporting columns supported between the upper bottom plate and the lower bottom plate; the upper base plate is provided with a pipe hole for inserting the purifying column, and the lower base plate is correspondingly provided with a limiting hole of the purifying column to position the purifying column.

7. The high-throughput dioxin sample pretreatment purification apparatus according to claim 6, characterized in that: the upper bottom plate is provided with a glass tube at the position of the tube hole.

Technical Field

The invention relates to the field of chemical analysis and biological research, in particular to an automatic pretreatment and purification device for a high-flux dioxin sample.

Background

Dioxin is a compound with strong carcinogenic, teratogenic and mutagenic effects, has strong toxicity (the international center for cancer research ranks the dioxin as human grade I carcinogen), and has the characteristics of difficult degradation and accumulation in organisms. Generally, dioxins refer to polychlorinated dibenzodioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) related in structure and chemical properties. Certain dioxin-like polychlorinated biphenyls (PCBs) have similar toxicity and are classified under the name of "dioxins". Approximately 419 dioxin-like compounds were identified, of which approximately 30 were considered to be quite toxic to dioxins, with 2,3,7,8-TCDD being the most toxic and typical persistent organic pollutants, ubiquitous in soil, water, atmosphere, and food and feed. Dioxin is easy to accumulate in organisms and seriously harms human bodies. The generation sources of dioxin are mainly two, namely, chemical substances including pesticides are manufactured; the second is from the incineration of the waste. Wherein, the chlorine-containing garbage is easy to generate dioxin due to incomplete combustion. Dioxin diffuses into the atmosphere along with smoke, and the human body breathes gas containing dioxin for a long time, which can cause serious influence on the body.

In the prior art, a dioxin detection technology is mainly isotope dilution-high resolution gas chromatography/high resolution magnetic mass spectrometry (HRGC/HRMS), and the method is already a gold standard of a dioxin determination standard (EPA1613 method), an european union dioxin determination standard (EN 1948:2006), a dioxin determination standard in chinese food (GB 5009.205-2013), a dioxin determination standard in chinese feed (GB/T28643-. The sample purification of isotope dilution-high resolution gas chromatography/high resolution magnetic mass spectrometry mainly adopts a manual method, comprises the steps of glass tube type selection, filler proportioning and filling, eluent addition, glass column movement to collect extracting solution and the like, is time-consuming and labor-consuming, and can cause serious reproducibility problems among different laboratories due to the influence of factors such as different experimenters, different material selection, different filling amounts and the like. The sample purification matched with the sample purification device in the market at present usually adopts equipment of American FMS company or Germany LCTech company, the principle is basically consistent, the solvent passes through the purification column through a pressure system, the system structure is complex, the blockage and the leakage are easy, the organic solvent consumption is large, and the simultaneous purification of a large number of samples cannot be realized.

Disclosure of Invention

The invention aims to solve the problems and provide a high-flux dioxin sample pretreatment purifying device. The method can automatically add the specified solvent into up to 20 purifying columns, synchronously complete the whole processes of purifying column leaching, column moving and extracting solution collecting, and realize high-flux and automatic purification of the dioxin sample.

In order to achieve the purpose, the technical scheme of the invention is as follows:

a high-flux dioxin sample pretreatment purifying device comprises a purifying column, a liquid feeding pipe, a spray pipe connected with the liquid feeding pipe, a detector for detecting the liquid level in the purifying column, a positioning and clamping device for fixing the spray pipe and the detector, and a transmission motion assembly for moving the positioning and clamping device to realize the movement of the positioning and clamping device in the X-axis direction, the Y-axis direction and the Z-axis direction; when the transmission motion assembly acts to enable the positioning and clamping device to be located above the glass column frame, the number and the position arrangement of the spray pipes clamped by the positioning and clamping device are consistent with those of the purification columns, liquid is added to the purification columns through the spray pipes, and the detector sequentially and circularly detects the height change of the liquid level in the purification columns.

As an improvement to the above technical scheme, the high-flux dioxin sample pretreatment purification device further comprises a solution bottle for providing a solution, and a liquid adding pump for pumping the solution in the solution bottle, wherein an outlet of the liquid adding pump is connected with a liquid adding pipe; the number of the solution bottles and the liquid adding pumps is matched with that of the liquid adding pipes.

As an improvement to the above technical solution, the transmission motion assembly includes an X-axis lead screw, an X-axis slider sleeved on the X-axis lead screw and driven by the X-axis lead screw to slide along the X-axis direction, a Z-axis lead screw penetrating through the X-axis slider and extending downward, a Z-axis slider fixed on the Z-axis lead screw and driven by the Z-axis lead screw to slide along the Z-axis direction, a Y-axis lead screw penetrating through the Z-axis slider and extending horizontally, and a Y-axis slider sleeved on the Y-axis lead screw and driven by the Y-axis lead screw to slide along the Y-axis direction, wherein the positioning and clamping device is fixed on the Y-axis slider.

As an improvement on the technical scheme, an X-axis motor is arranged at one end of the X-axis lead screw, a Z-axis motor is arranged at one end of the Z-axis lead screw, and a Y-axis motor is arranged at one end of the Y-axis lead screw.

As an improvement to the above technical solution, the positioning and clamping device is a fixed plate, and the fixed plate is provided with a plurality of insertion holes for insertion of the spray pipe and the detector; one of the jacks is used for inserting the detector, and the other jacks are used for inserting the spray pipe.

As an improvement to the above technical solution, the high-flux dioxin sample pretreatment purification device further comprises a glass column frame for inserting purification columns, wherein the glass column frame comprises a lower base plate, an upper base plate and support columns supported between the upper base plate and the lower base plate; the upper base plate is provided with a pipe hole for inserting the purifying column, and the lower base plate is correspondingly provided with a limiting hole of the purifying column to position the purifying column.

As an improvement to the technical scheme, the upper bottom plate is provided with a glass tube at the position of the tube hole.

The working principle of the high-flux dioxin sample pretreatment purifying device is as follows:

the X slide block, the Y slide block and the Z slide block can move along corresponding slide bars (the X slide bar, the Y slide bar and the Z slide bar) to drive the spray pipe positioning and clamping device to move above any one purification column, and the purification columns are positioned through the column box. After the liquid adding pump is started, liquid is added to the purification column from the solution bottle through the liquid adding pipe. The device can be additionally provided with a control device to control the X slide block, the Y slide block, the Z slide block and the liquid adding pump, so that one or more kinds of liquid can be automatically added into one or more purification columns at regular time and quantity.

Compared with the prior art, the invention has the advantages and positive effects that:

the high-flux dioxin sample pretreatment purifying device can automatically add specified solvent into up to 20 purifying columns, synchronously complete the operations of purifying column leaching, column moving and extracting solution collecting, and realize high-flux full-automatic purification of dioxin samples.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.

FIG. 1 is a front view structural diagram of the present invention;

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.

As shown in fig. 1, the high-flux dioxin sample pretreatment purifying device of the invention comprises a purifying column 9, a liquid adding pipe 10, a spray pipe 14 connected with the liquid adding pipe 10, a detector 11 for detecting the liquid level in the purifying column 9, a positioning and clamping device 7 for fixing the spray pipe 14 and the detector 11, and a transmission motion assembly for moving the positioning and clamping device 7 to realize the movement in the directions of an X axis, a Y axis and a Z axis; when the transmission motion assembly acts to enable the positioning and clamping device 7 to be located above the glass column frame, the number and the position arrangement of the spray pipes 14 clamped by the positioning and clamping device 7 are consistent with those of the purifying columns 9, liquid is added to the purifying columns 9 through the spray pipes 14, and the detector 11 sequentially and circularly detects the height change of the liquid level in the purifying columns 9.

The high-flux dioxin sample pretreatment purifying device further comprises a solution bottle 12 for providing solution and a liquid adding pump 13 for pumping the solution in the solution bottle 12, wherein an outlet of the liquid adding pump 13 is connected with a liquid adding pipe 10; the number of the solution bottles 12 and the liquid adding pumps 13 is matched with that of the liquid adding pipes 10.

The transmission motion assembly comprises an X-axis lead screw 1, a X-axis slide block 2 driven by the X-axis lead screw 1 to slide along the X-axis direction is sleeved on the X-axis lead screw 1, a Z-axis lead screw 3 extending downwards and arranged on the X-axis slide block 2 is penetrated, the Z-axis slide block 4 driven by the Z-axis lead screw 3 to slide along the Z-axis direction is fixed on the Z-axis lead screw 3, a Y-axis lead screw 5 extending along the Z-axis direction is penetrated and arranged on the Z-axis slide block 4 and the horizontal direction, the Y-axis slide block 6 driven by the Y-axis lead screw 5 to slide along the Y-axis direction is sleeved on the Y-axis lead screw 5, and the positioning and clamping device. One end of the X-axis lead screw 1 is provided with an X-axis motor 16, one end of the Z-axis lead screw 3 is provided with a Z-axis motor 17, and one end of the Y-axis lead screw 5 is provided with a Y-axis motor 15.

The spray pipe positioning and clamping device 7 is a fixed plate, and the fixed plate is provided with a plurality of insertion holes for inserting the spray pipe 14 and the detector 11; one of which is for insertion of the probe 11 and the remaining of which is for insertion of the nozzle 14. Except the jacks for inserting the detector 11, the number and the position arrangement of the other jacks are consistent with those of the purification columns.

The high-flux dioxin sample pretreatment purifying device also comprises a glass column frame for inserting purifying columns, wherein the glass column frame comprises a lower bottom plate, an upper bottom plate and supporting columns supported between the upper bottom plate and the lower bottom plate; the upper base plate is provided with a pipe hole for inserting the purifying column, and the lower base plate is correspondingly provided with a limiting hole of the purifying column to position the purifying column. The upper plate is provided with glass tubes 18 at the locations of the tube holes.

The working principle of the high-flux dioxin sample pretreatment purifying device is as follows:

the X slide block, the Y slide block and the Z slide block can move along corresponding slide bars (the X slide bar, the Y slide bar and the Z slide bar) to drive the spray pipe positioning and clamping device to move above any one purification column, and the purification columns are positioned through the column box. After the liquid adding pump is started, liquid is added to the purification column from the solution bottle through the liquid adding pipe. Can increase and set up controlling means and control X slider, Y slider, Z slider, liquid feeding pump, realize adding 1 or multiple liquid to 1 or many clean columns automatic timing ration.

According to the high-flux dioxin sample pretreatment purification device, the designated solvent can be added into the purification columns, and the work of washing, transferring and collecting the extracting solution of the purification columns is completed, so that the high-flux purification of the dioxin sample is realized.