WO2021227546A1 - Chemin d'écoulement et procédé d'extraction d'échantillon multifonctionnel - Google Patents

Chemin d'écoulement et procédé d'extraction d'échantillon multifonctionnel Download PDF

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Publication number
WO2021227546A1
WO2021227546A1 PCT/CN2021/071354 CN2021071354W WO2021227546A1 WO 2021227546 A1 WO2021227546 A1 WO 2021227546A1 CN 2021071354 W CN2021071354 W CN 2021071354W WO 2021227546 A1 WO2021227546 A1 WO 2021227546A1
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WO
WIPO (PCT)
Prior art keywords
valve
rotary valve
channel
solenoid valve
sample
Prior art date
Application number
PCT/CN2021/071354
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English (en)
Chinese (zh)
Inventor
林春生
戴相辉
陈克彦
郭宝辉
林志杰
Original Assignee
睿科集团(厦门)股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from CN202010395244.XA external-priority patent/CN111437626A/zh
Priority claimed from CN202020772149.2U external-priority patent/CN212491678U/zh
Application filed by 睿科集团(厦门)股份有限公司 filed Critical 睿科集团(厦门)股份有限公司
Publication of WO2021227546A1 publication Critical patent/WO2021227546A1/fr

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/14Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography
    • B01D15/10Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/20Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material

Definitions

  • priority number 202010395244.X priority date 2020-5-12
  • priority number 202020772149.2 priority date 2020-5-12
  • the invention relates to the technical field of experimental extraction, in particular to a multifunctional sample extraction flow path and method.
  • the purpose of the present invention is to provide a multifunctional sample extraction flow path and method, which can realize the continuity and automatic extraction operation of small-volume or large-volume samples, and improve the extraction efficiency and convenience.
  • the solution of the present invention is: a multi-channel sample extraction flow path, including a multi-channel solenoid valve, a rotary valve, a syringe, a collection tube, an SPE column, a waste tank, a sample bottle, and the multi-channel solenoid valve
  • the valve is provided with a variety of solvent channels controlled by solenoid valves.
  • the rotary valve includes No. 0 position, No. 1 position, No. 2 position, No. 3 position and No. 4 position.
  • Position and position 4 are distributed on the outer edge of the rotary valve, the position 0 is set in the middle of the rotary valve, the syringe is connected to position 0, the collection tube is connected to position 1, and the outlet of the multi-channel solenoid valve is connected to 2.
  • the inlet of the SPE column is connected to No. 3
  • the outlet of the SPE column can choose to flow to a collection tube or a waste discharge tank, and the sample bottle is connected to No. 4;
  • the rotary valve is provided with a radial channel, The number 0 position and each number position are communicated with each other through the radial channel.
  • the rotary valve is further provided with an edge channel, the edge channel is arranged on the side of the outer end of the radial channel, and the edge channel is used to connect two adjacent numbers on the edge of the rotary valve.
  • the rotary valve adopts a three-turn twelve-way valve
  • the three-turn twelve-way valve includes three sets of indexing positions, and each set of indexing positions includes a 0 position, a 1 position, a second position, A No. 3 position, a No. 4 position, a radial channel and an edge channel, a total of twelve positions, three radial channels and three edge channels, the three sets of indexing rings are evenly distributed on the rotary valve .
  • the multi-channel solenoid valve is also provided with a nitrogen channel controlled by the solenoid valve, the nitrogen channel is connected to the sample bottle, and the three-way solenoid valve is arranged between the nitrogen channel and the sample bottle .
  • a multifunctional sample extraction method including the following steps:
  • the concentration step can be performed after the elution step, and the collection tube is externally provided with a nitrogen pipeline controlled by a two-way solenoid valve.
  • the two-way solenoid valve is opened, and the nitrogen gas can pass through the two-way solenoid valve.
  • the solenoid valve is blown directly onto the liquid surface of the collection tube to concentrate until the concentration reaches the specified volume.
  • the dissolution step can be performed after the elution step.
  • the rotary valve is rotated, and the rotary valve is switched to position 0 to communicate with position 2.
  • the valve selects the required solvent and aspirates the liquid, then rotates the rotary valve again, and the rotary valve switches to position 0 to communicate with position 1.
  • the syringe pushes the liquid, and the required solvent is directly dropped into the collection tube through the No. 1 port to complete the transfer.
  • the multi-channel solenoid valve of the extraction flow path can be loaded with a variety of solvents required for extraction, which is convenient for uniformly replenishing various solvents.
  • the solvents include activators, eluents, eluents, etc. Wait.
  • the radial channel on the rotary valve in this case is a channel extending from the middle to the edge, so the switching rotary valve can control the central position 0 and the edge positions (position 1, position 2, position 3, and position 4).
  • the degree of automation is more obvious, which improves the inconvenience of the existing solid phase extraction instrument and improves Extraction efficiency.
  • FIG. 1 is a schematic diagram of the structure of the first state of an embodiment of the present invention.
  • Fig. 2 is a schematic structural diagram of a second state of an embodiment of the present invention.
  • Fig. 3 is a schematic structural diagram of the third state of an embodiment of the present invention.
  • Fig. 4 is a schematic structural diagram of a fourth state of an embodiment of the present invention.
  • Fig. 5 is a schematic structural diagram of a fifth state of an embodiment of the present invention.
  • Multi-channel solenoid valve 10 solvent channel 101, nitrogen channel 102, air channel 103, rotary valve 20, radial channel 201, edge channel 202, syringe 30, collection tube 40, SPE column 50, waste tank 60, sample bottle 70 , Three-way solenoid valve 80, two-way solenoid valve 90, nitrogen pipeline 901.
  • the present invention provides a multifunctional sample extraction flow path, as shown in Figure 1, comprising a multi-channel solenoid valve 10, a rotary valve 20, a syringe 30, a collection tube 40, an SPE column 50, a waste tank 60, a sample bottle 70, three Two-way solenoid valve 80 and a two-way solenoid valve 90.
  • the multi-channel solenoid valve 10 is provided with multiple solvent channels 101 controlled by the solenoid valve.
  • the rotary valve 20 includes No. 0 position, No. 1 position, No. 2 position, 3 No. and No. 4 positions, the No. 1, No. 2, No. 3 positions, and No. 4 positions are distributed on the outer edge of the rotary valve 20, the No.
  • 0 position is arranged in the middle of the rotary valve 20, and the syringe 30 is connected to 0 No. 1, the collection tube 40 is connected to the No. 1, the outlet of the multi-channel solenoid valve 10 is connected to the No. 2, the inlet of the SPE column 50 is connected to the No. 3, and the outlet of the SPE column 50 can select the flow direction to collect The tube 40 or the waste tank 60, the sample bottle 70 is connected to the 4th position.
  • the multi-channel solenoid valve 10 in this case can be loaded with a variety of solvents required for extraction, which is convenient for uniformly replenishing various solvents.
  • the solvents include activators, eluents, eluents, and so on.
  • the rotary valve 20 is provided with a radial channel 201 and an edge channel 202, and the diameter is passed between the 0 position and the other positions (position 1, position 2, position 3, and position 4). It is connected to the channel 201, and the edge channel 202 is arranged on the side of the outer end of the radial channel 201.
  • the edge channel 202 is used to connect the two adjacent positions of the edge of the rotary valve 20 (position 1, position 2, and position 2). And position 3, position 3 and position 4).
  • the rotary valve 20 adopts a three-turn twelve-way valve.
  • the three-turn twelve-way valve includes three sets of indexing positions. Number position, a number position, a radial channel 201 and an edge channel 202, a total of twelve number positions, three radial channels 201 and three edge channels 202, the three sets of indexing rings are evenly distributed in the rotation
  • the valve 20 is on.
  • the number position mentioned in this case means the gear position.
  • position 1 is the first gear position
  • position 2 is the second gear position....
  • the position 0 is set at the rotary valve 20 Therefore, in the fan-shaped active area of each group of indexing, the 0 position is basically kept in the middle.
  • the outer end of the radial channel 201 continuously changes to communicate with other positions, and the radial channel 201 The inner end is connected to position 0, so as to realize the communication combination of the syringe 30 and the instrument, and obtain the combined effect of different flow paths.
  • the present invention also provides a multifunctional sample extraction method, including the following steps:
  • the SPE column 50 is activated, the sample is loaded into the sample bottle 70, the sample bottle 70 is capped, and then turned upside down.
  • the rotary valve 20 is rotated.
  • the rotary valve 20 communicates with No. 0 through the radial channel 201 Position and position 2 (state 2), the syringe 30 selects the activator from the multi-channel solenoid valve 10 through the No. 2 port, and sucks the liquid, then rotates the rotary valve 20 again, and the rotary valve 20 switches to the position 0 to connect to the position 3 (state (3)
  • the syringe 30 pushes the liquid, and the solvent pushes the activator through the SPE column 50 to the waste tank 60 through the No. 3 port, and repeats this process to complete the activation of the activated SPE column 50.
  • the multi-channel solenoid valve 10 is also provided with a nitrogen channel 102 and an air channel 103 controlled by a solenoid valve, the nitrogen channel 102 is connected to the sample bottle 70, and the three-way solenoid valve 80 is arranged between the nitrogen channel 102 and the sample bottle 70 between.
  • the existing solid phase extraction instrument cannot pass the column quickly and continuously.
  • the present invention can realize the positive pressure auxiliary syringe 30 sample loading and the positive pressure rapid sample loading to achieve the purpose of accelerating the sample loading speed.
  • the sample loading process of the positive pressure auxiliary syringe 30 is specifically as follows: first rotate the rotary valve 20. With reference to Figs.
  • the rotary valve 20 communicates with position 0 and position 4 (state 4) through a radial channel 201.
  • three The solenoid valve 80 opens the NC COM port, and nitrogen can flow from the nitrogen channel 102 to the sample bottle 70.
  • Positive pressure is generated in the sample bottle 70 to accelerate the suction speed of the syringe 30, and then switch the rotary valve to position 0 and connect to position 3.
  • State 3 the syringe 30 pushes the liquid, and the sample can pass through the SPE column 50 to the waste tank 60 for sample loading.
  • the positive pressure auxiliary syringe 30 is suitable for sample loading with high density or low boiling point, which cannot be loaded quickly and needs to be loaded stably.
  • the operation process of the positive pressure rapid sample loading is specifically as follows: first rotate the three-turn twelve-way valve, as shown in FIG.
  • the three-way solenoid valve 80 opens the NC port COM, nitrogen can flow from the nitrogen channel 102 to the sample bottle 70, generate positive pressure in the sample bottle 70, and then directly positive pressure to the SPE column 50 (membrane), and finally to the waste tank 60.
  • the positive pressure rapid sample loading does not need to pass through the syringe 30, and is suitable for samples that require very fast loading, such as membrane extraction.
  • the rinsing step and the elution step there is also a drying step of the SPE column 50.
  • the process of this step is to rotate the rotary valve 20. As shown in FIG. 4, the rotary valve 20 passes through the edge channel 202. Connect No. 2 and No. 3 positions (state 4). At this time, open the nitrogen channel 102 of the multi-channel solenoid valve, and the nitrogen can pass through the 2nd-3rd-SPE column 50 for nitrogen blowing to dry the SPE Column 50 packing effect.
  • a concentration step can be performed after the elution step.
  • the collection tube 40 is externally provided with a nitrogen pipeline 901 controlled by a two-way solenoid valve 90. After the SPE column 50 is eluted, the two-way solenoid valve is turned on. Valve 90, the nitrogen can be blown directly onto the liquid surface of the collection pipe 40 through the two-way solenoid valve 90 for concentration until the concentration reaches the specified capacity.
  • the dissolution step can be performed after the elution step.
  • the rotary valve 20 is rotated.
  • the rotary valve 20 is switched to position 0 to communicate No. 2 position (state 2), the syringe 30 selects the required solvent from the multi-channel solenoid valve 10 through the No. 2 port, and sucks the liquid, and then rotates the rotary valve 20 again, and the rotary valve 20 switches to the 0th position and connects to the 1st position (state 1)
  • the syringe 30 pushes the liquid, and drops the required solvent directly into the collection tube 40 through the No. 1 port to complete the transfer.
  • the extraction flow path can realize the extraction action of SPE column activation-multi-function loading-rinsing-SPE column drying-elution-dissolution or concentration at one time.
  • the radial channel 201 on the rotary valve 20 is from the middle to the The edge extension channel
  • the edge channel 202 is a channel with two adjacent positions on the edge. Therefore, the switching rotary valve 20 can control the central position 0 and the edge positions (position 1, position 2, position 3, and position 4). It can also connect to position 1 and position 2 (state 3), position 2 and position 3 (state 4), position 3 and position 4 (state 5), and then flexibly change the communication channel
  • the sequence of operations can realize continuous extraction operations for small-volume samples or large-volume samples.
  • the degree of automation is more obvious, which improves the inconvenience of the existing solid phase extraction instrument and improves the extraction efficiency.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

Un chemin d'écoulement d'extraction d'échantillon multifonctionnel, comprenant une électrovanne à canaux multiples (10), une vanne rotative (20), un injecteur (30), un tube de collecte (40), une colonne SPE (50), un réservoir de décharge de déchets (60), et une bouteille d'échantillon (70). L'électrovanne à canaux multiples (10) est pourvue d'une pluralité de canaux de solvant commandés par l'électrovanne ; la vanne rotative (20) comprend des positions 0, des positions 1, des positions 2, des positions 3 et des positions 4 ; les positions 1, les positions 2, les positions 3 et les positions 4 sont réparties sur le bord de la vanne rotative (20), et les positions 0 sont agencées au milieu de la vanne rotative (20) ; l'injecteur (30) est relié à une position 0 ; le tube de collecte (40) est reliée à une position 1 ; la sortie de l'électrovanne à canaux multiples (10) est reliée à une position 2 ; l'entrée de la colonne SPE (50) est reliée à une position 3 ; la sortie de la colonne SPE (50) peut guider sélectivement vers le tube de collecte (40) ou le réservoir de décharge de déchets (60) ; la bouteille d'échantillon (70) est reliée à une position 4 ; la vanne rotative (20) est pourvue de canaux radiaux, et les positions 0 sont en communication avec les autres positions au moyen des canaux radiaux. Selon le chemin d'écoulement d'extraction, l'opération d'extraction continue et automatique de petits échantillons de petit volume ou de grand volume peut être mise en œuvre, et l'efficacité d'extraction et la commodité sont améliorées.
PCT/CN2021/071354 2020-05-12 2021-01-13 Chemin d'écoulement et procédé d'extraction d'échantillon multifonctionnel WO2021227546A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
CN202020772149.2 2020-05-12
CN202010395244.XA CN111437626A (zh) 2020-05-12 2020-05-12 一种多功能样品萃取流路及方法
CN202010395244.X 2020-05-12
CN202020772149.2U CN212491678U (zh) 2020-05-12 2020-05-12 一种多功能样品萃取流路

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WO2021227546A1 true WO2021227546A1 (fr) 2021-11-18

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202522549U (zh) * 2012-04-16 2012-11-07 北京莱伯泰科仪器有限公司 一种全自动黄曲霉毒素分析系统
CN206594116U (zh) * 2016-10-21 2017-10-27 杭州职业技术学院 一种用于pm2.5中多环芳烃样品的自动前处理装置
WO2018059639A1 (fr) * 2016-09-28 2018-04-05 Evosep Aps Analyse chromatographique à refocalisation de gradient double à basse pression
EP3386628B1 (fr) * 2016-02-29 2019-06-12 Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Dispositif à écoulement continu modulaire
CN110393945A (zh) * 2019-09-04 2019-11-01 睿科集团(厦门)股份有限公司 一种多通道加压萃取流路及其萃取方法
CN111060609A (zh) * 2019-12-06 2020-04-24 厦门大学 一种全自动固相萃取富集的分析装置和分析方法
CN111437626A (zh) * 2020-05-12 2020-07-24 睿科集团(厦门)股份有限公司 一种多功能样品萃取流路及方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN202522549U (zh) * 2012-04-16 2012-11-07 北京莱伯泰科仪器有限公司 一种全自动黄曲霉毒素分析系统
EP3386628B1 (fr) * 2016-02-29 2019-06-12 Max-Planck-Gesellschaft zur Förderung der Wissenschaften e.V. Dispositif à écoulement continu modulaire
WO2018059639A1 (fr) * 2016-09-28 2018-04-05 Evosep Aps Analyse chromatographique à refocalisation de gradient double à basse pression
CN206594116U (zh) * 2016-10-21 2017-10-27 杭州职业技术学院 一种用于pm2.5中多环芳烃样品的自动前处理装置
CN110393945A (zh) * 2019-09-04 2019-11-01 睿科集团(厦门)股份有限公司 一种多通道加压萃取流路及其萃取方法
CN111060609A (zh) * 2019-12-06 2020-04-24 厦门大学 一种全自动固相萃取富集的分析装置和分析方法
CN111437626A (zh) * 2020-05-12 2020-07-24 睿科集团(厦门)股份有限公司 一种多功能样品萃取流路及方法

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