WO2023072317A1 - Device for multi-channel electrochemical measuring and method of use thereof - Google Patents

Device for multi-channel electrochemical measuring and method of use thereof Download PDF

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Publication number
WO2023072317A1
WO2023072317A1 PCT/CZ2021/050119 CZ2021050119W WO2023072317A1 WO 2023072317 A1 WO2023072317 A1 WO 2023072317A1 CZ 2021050119 W CZ2021050119 W CZ 2021050119W WO 2023072317 A1 WO2023072317 A1 WO 2023072317A1
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WO
WIPO (PCT)
Prior art keywords
electrode systems
lid
row
reaction wells
plate
Prior art date
Application number
PCT/CZ2021/050119
Other languages
French (fr)
Inventor
Aleš DAŇHEL
Lukáš FOJT
Miroslav FOJTA
Original Assignee
Biofyzikální Ústav Akademie Věd České Republiky
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Priority to PCT/CZ2021/050119 priority Critical patent/WO2023072317A1/en
Publication of WO2023072317A1 publication Critical patent/WO2023072317A1/en

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • B01L3/5085—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates
    • B01L3/50853—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates with covers or lids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/04—Closures and closing means
    • B01L2300/041—Connecting closures to device or container
    • B01L2300/043—Hinged closures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/04—Closures and closing means
    • B01L2300/046—Function or devices integrated in the closure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/06—Auxiliary integrated devices, integrated components
    • B01L2300/0627—Sensor or part of a sensor is integrated
    • B01L2300/0645—Electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0809—Geometry, shape and general structure rectangular shaped
    • B01L2300/0829—Multi-well plates; Microtitration plates
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis

Definitions

  • the invention relates to a device for multi-channel electrochemical measuring for performing a variety of electrochemical measurements within one plate comprising a plurality of reaction wells.
  • Another known arrangement uses multi-channel layered multi-electrodes, which are characterised by an arrangement of working electrodes in close proximity to the reference and auxiliary electrodes (i.e., all working electrodes share the auxiliary and reference electrodes).
  • this solution also allows measurements in only one solution and does not allow simultaneous measurement of multiple samples.
  • a disadvantage of the above solutions is the need for large amount of the analysed sample, complex design of the device, and large number of the electrode systems, which corresponds to the number of wells of the microtiter plate with the samples. For different types of measurements within one microtiter plate, manual pipetting and other steps are often required, which greatly complicate the electrochemical measurements and increase the risk of human error.
  • Another disadvantage is that they do not allow measurements without the presence of oxygen in the measured solution.
  • the above shortcomings are eliminated to a certain extent by a device for multichannel electrochemical measuring of the present invention.
  • the device for multi-channel electrochemical measuring comprises a bottom portion, a lid, and a plate comprising a plurality of reaction wells for measured samples, wherein the lid comprises a plurality of the electrode systems.
  • the bottom portion of the device is movably connected to the lid and comprises a cavity for receiving the plate, wherein the lid has a first position, in which all electrode systems are located outside the reaction wells, and a second position, in which all electrode systems are located at least partially inside the reaction wells.
  • the electrode systems on the lid are arranged in at least one row of the electrode systems, and the reaction wells are arranged in parallel rows of the reaction wells, wherein each row of the reaction wells comprises a number of reaction wells corresponding to the number of the electrode systems in the at least one row of the electrode systems, and the number of rows of the reaction wells is greater than the number of rows of the electrode systems.
  • the rows of the electrode systems are parallel to the rows of the reaction wells, and the plate is slidably movably connected to the bottom portion in a direction perpendicular to the at least one row of the electrode systems.
  • An advantage of the device of the invention lies in particular in the combination of the adjustable sliding movement of the plate with a plurality of reaction wells and the specific arrangement of the electrode systems, which allows the use of a single row of the electrode systems for different electrochemical measurements in rows of reaction wells within one plate, or alternatively, a row of the wells can be used to wash the electrode systems or to modify their surface.
  • the lid comprises just one row of the electrode systems placed on the underside of the lid along the edge of the lid from the underside of the lid. Placing the electrode systems in only one row saves electrode systems, wherein measurements in all rows of the reaction wells on the plate are made with one row of the electrode systems.
  • the lid is rotatably movably connected to the bottom portion by its first end and comprises a row of the electrode systems at its second end along the free edge of the lid, wherein the first end of the lid and the second end of the lid are located on the opposite sides of the lid.
  • the plate comprising a plurality of the reaction wells preferably comprises at least 6 rows of the reaction wells, and each row comprises at least 8 reaction wells, wherein the number of rows of the reaction wells is at least twice the number of rows of the electrode systems.
  • the bottom portion of the device of the invention comprises a stop for fixing the position of the plate.
  • the stop is adjustable and serves for securing the plate such that when the lid of the electrode system is in the second position, it is at least partially inside the reaction wells of the respective row of the reaction wells on the plate.
  • the device for multi-channel electrochemical measuring further preferably comprises arresting of the lid.
  • the depth of immersion of the electrode systems into the reaction wells on the plate can be regulated, or the analysis can be performed only on a drop of the measured sample.
  • the arresting of the lid then ensures that the lid is fixed in position.
  • the electrode systems are removably connected to the lid, wherein the electrode systems comprise a carrier and the lid comprises connectors adapted to removably connect the carrier of the electrode systems, wherein at least 2 electrode systems in one row of the electrode systems share a common carrier.
  • the lid comprises a plurality of capillaries for supplying an auxiliary medium to the electrode systems in the vicinity of the electrode systems, wherein each capillary is in the second position of the lid located at least partially within a reaction well in which the electrode system is also at least partially located.
  • the capillaries for supplying the auxiliary medium can be used, for example, to saturate or bubble the sample in the reaction wells with auxiliary gas before or during the electrochemical measurement. This also enables performing electrochemical measurements without the presence of oxygen on the electrode system.
  • a preferred method of using the device for multi-channel electrochemical measuring comprises the following steps: when the lid is opened, the plate is inserted into the cavity for receiving the plate, and then the lid is closed, thereby bringing the first row of the electrode systems into a position where all the electrode systems of the first row of the electrode systems are at least partially located within the reaction wells of the first row of the reaction wells.
  • the first row of the electrode systems When the lid is reopened, the first row of the electrode systems is brought to a position where all the electrode systems of the first row of the electrode systems are outside the reaction wells and subsequently the plate is displaced relative to the bottom portion perpendicular to the first row of the electrode systems, wherein after the lid is subsequently closed, the first row of the electrode systems is brought into a position where all the electrode systems of the first row of the electrode systems are at least partially located inside the reaction wells of the second row of the reaction wells, wherein the plate comprises both the first row of the reaction wells and the second row of the reaction wells.
  • fig. 1 shows a section through the device for multi-channel electrochemical measuring of the invention with the lid placed in the second position
  • fig. 2 shows a front view of the device for multi-channel electrochemical measuring of the invention with the lid placed in the first position
  • fig. 3 shows a section through the electrode system when immersed in the reaction well
  • fig. 4a shows an embodiment of one carrier for one electrode system
  • fig. 4b shows an embodiment of one carrier for 4 electrode systems
  • fig. 4c shows an embodiment of one carrier for 8 electrode systems.
  • One exemplary embodiment is a structure of the device for multi-channel electrochemical measuring of the invention shown in figs. 1 and 2.
  • the structure of the device for multi-channel electrochemical measuring of the exemplary embodiment comprises a bottom portion 1_, a lid 2, and a plate 3 comprising a plurality of reaction wells 4, wherein the lid 2 comprises precisely one row of the electrode systems 5.
  • the bottom portion 1. has the shape of a plate, wherein the bottom portion 1. comprises a cavity adapted for inserting the plate 3 with a plurality of the reaction wells 4 which opens on the top side of the bottom portion 1_.
  • the plate 3 with plurality of the reaction wells 4 is, in this exemplary embodiment, a standard microtiter plate with 96 reaction wells 4 comprising 12 rows of the reaction wells 4, wherein each row of the reaction wells 4 comprises 8 reaction wells 4.
  • the plate 3 is slidably movably disposed on the bottom portion 1_ and slidable in the plane of the upper surface of the bottom portion 1. in a direction perpendicular to the row of the electrode systems 5 attached to the lid 2.
  • the plate 3 has a first position where all electrode systems 5 of the row of the electrode systems 5 are at least partially located inside the reaction wells 4 of the first (outermost) row of the reaction wells 4, and a second position where all electrode systems 5 of the row of the electrode systems 5 are located at least partially inside the reaction wells 4 of the second row of the reaction wells 4 of the plate 3.
  • the bottom portion 1_ comprises a passageway in the wall opening into the cavity through which the plate 3 can be slid in and out, wherein the cavity comprises guide grooves enabling movement of the plate 3 in a direction perpendicular to the row of the electrode systems 5 while preventing movement of the plate 3 in a direction parallel to the row of the electrode systems 5.
  • the bottom portion 1. of the device further comprises an adjustable stop 6 for fixing the position of the plate 3.
  • the lid 2 in the first exemplary embodiment has the shape of a plate rotatably movably connected to the bottom portion 1_, wherein the connection of the lid 2 to the bottom portion 1. is located at the first end of the lid 2.
  • the lid 2 comprises a row of the electrode systems 5, wherein the first end of the lid 2 and the second end of the lid 2 are located on opposite sides of the lid 2.
  • the lid 2 comprises electrode systems 5 arranged in precisely one row of the electrode systems 5, wherein the row of the electrode systems 5 is placed on the underside of the lid 2 along the free edge of the lid 2 at a distance of 2 to 10 mm, preferably 3 to 6 mm from the margin of the free edge of the lid 2.
  • the lid 2 has a first position in which all electrode systems 5 of the row of the electrode systems 5 are located outside the reaction wells 4 of the plate 3 (view of the device of fig. 2), and a second position in which all electrode systems 5 of the row of the electrode systems 5 are located at least partially inside the reaction wells 4 belonging to the first (outermost) row of the reaction wells 4 of the plate 3 (section through the device of fig. 1 ).
  • the direction of the movement of the lid 2 during opening is shown by the corresponding arrow in fig. 1 .
  • the definition of the sliding movement of the plate 3 in the direction perpendicular to the row of the electrode systems 5 relates to the placement of the lid 2 in the second position.
  • the lid 2 of the device for multi-channel electrochemical measuring comprises, on the side adjacent to the bottom portion 1_, a plurality of connectors 9 placed in a row along the free edge of the lid 2, adapted for connecting and securing the carriers 8 of the electrode systems 5.
  • the electrode systems 5 are layered electrode systems.
  • This exemplary embodiment of the device of the invention comprises a total of 8 connectors 9, where the carrier 8 of the electrode systems 5 with one or more electrode systems 5 may be connected to each connector 9. Possible arrangements of the electrode systems 5 on the carrier 8 of the electrode systems 5 will be further described in alternative embodiments according to the present invention with reference to figs. 4a-4c. All connectors 9 for the carriers 8 of the electrode systems 5 are connected through an electric line to the output connector 11 connecting the device for multi-channel electrochemical measuring of the present invention with a measuring device, e.g., a multichannel potentiostat.
  • capillaries 10 for supplying the auxiliary medium from the auxiliary medium source 12 are placed on the lid 2 in a row in front of or behind the connectors 9 or the carriers 8 of the electrode systems 2.
  • the auxiliary medium source 12 is, in the first exemplary embodiment, any auxiliary or inert gas, e.g., nitrogen or argon.
  • the capillary 10 for supplying the auxiliary medium has a tapered mouth directed towards the surface of the electrode system 5 and allows saturation or bubbling of the analysed sample in the reaction well 4 with the selected gas or removal of oxygen from the analysed sample before or during the electrochemical measurement.
  • the capillaries 10 for the auxiliary medium are located at least partially inside the reaction wells 4.
  • the electrode systems 5 are at least partially immersed in the respective reaction wells 4, this detail is shown in fig. 3.
  • the depth of immersion of the electrode systems 5 into the reaction wells 4 is regulated by movement of the lid 2.
  • the lid 2 is rotatably movably connected to the bottom portion 1_, wherein the vertical position of the electrode systems 5 can be adjusted by moving the lid 2, and the position of the lid 2 can be arrested using an arresting screw placed on the pivot pin of the lid 2.
  • electrochemical measurements can be made also for samples with extremely small volumes or in a single drop (at least 3 pL) of the analysed sample applied on each carrier 8 of the electrode system 5 at the location of the electrode system 5.
  • the method of use of the device for multi-channel electrochemical measuring of an exemplary embodiment comprises the following consecutive steps:
  • steps 5 and 6 may be performed in steps 5 and 6 according to the above method of use of the device.
  • the analysed sample or an auxiliary substance e.g., a cleaning solution, may be placed in the entire selected rows of wells 4, wherein the row of wells 4 may be used, e.g., for rinsing the electrode systems 5, modifying the electrode systems 5, or for interaction studies.
  • the above steps may include the steps of fixing the position of the plate 3 by means of the stop 6 or readjusting the position of the lid 2 and its subsequent arresting 7.
  • the method of use of the device of the first exemplary embodiment of the invention preferably enables saturation or bubbling of the analysed sample in the reaction well 4 with a selected auxiliary gas (e.g., nitrogen, argon) or removing oxygen from the analysed sample before or during the electrochemical measurement.
  • a selected auxiliary gas e.g., nitrogen, argon
  • the gas supply from the auxiliary medium source 12 to the capillaries 10 for supplying the auxiliary medium can be opened and closed before or at any time during the electrochemical measurement.
  • the lid 2 may comprise multiple rows of the electrode systems 5, e.g., precisely two parallel rows of the electrode systems 5.
  • the first row of the electrode systems 5 is positioned on the underside of the lid 2 along the free edge of the second end of the lid 2 as in the first exemplary embodiment of the device of the invention, wherein the second row of the electrode systems 5 is positioned on the underside of the lid 2 parallel to the first row of the electrode systems 5.
  • the plate 3 in this embodiment is also a 96-well microtiter plate.
  • the gap, or distance, between the first row of the electrode systems 5 and the second row of the electrode systems 5 corresponds to a multiple of the width of one row of the reaction wells 4, wherein in this embodiment, this gap between the rows of the electrode systems 5 corresponds to a multiple of 5 times the width of the row of the reaction wells 4, wherein, in the first position of the plate 3 and the second position of the lid 2, the first row of the electrode systems 5 is at least partially located inside the first (outermost) row of the reaction wells 4 and, at the same time, the second row of the electrode systems 5 is at least partially located inside the seventh row of the reaction wells 4 on the plate 3.
  • the first row of the electrode systems 5 is located at least partially inside the second row of the reaction wells 4, and at the same time, the second row of the electrode systems 5 is at least partially inside the eighth row of the reaction wells 4 on the plate 3.
  • the first row of the electrode systems 5 may be located at least partially inside the first (outermost) to sixth row of the reaction wells 4 during the measurement throughout the entire plate 3, and the second row of the electrode systems 5 may be located continuously at least partially inside the seventh to twelfth row of the reaction wells 4. Electrochemical measurement, optionally rinsing, and other procedures can thus be carried out in two rows of the reaction wells 4 simultaneously. Some rows of the reaction wells can be used to clean or modify the electrode surface.
  • Another possible embodiment of the device of the invention comprises the same method of movably connecting the lid 2 to the bottom portion 1. as in the first exemplary embodiment, differing only in the position of the rotatable connection of the lid 2 to the bottom portion 1_.
  • the rotatable connection of the lid 2 to the bottom portion 1. may be located at any lateral edge of the lid 2 between the first end and the second end of the lid 2, wherein the axis of rotation of the rotatable connection is parallel to the direction of movement of the plate 3.
  • the rows of the electrode systems 5 must still be oriented perpendicularly to the movement of the plate 3 in the second position of the lid 2.
  • Alternative embodiments of the device of the invention may include other options of movable connection and mutual orientation of the bottom portion 1_ and the lid 2.
  • Any suitable mechanical, hydraulic, pneumatic, or combined lifting system e.g., parallelogram, screwjack, scissor jack, piston jack, etc., can be used to height-adjust and move the lid 2.
  • Other possible embodiments of the invention may include various types of plates 3 having a plurality of the reaction wells 4 varying in the number of the reaction wells 4 in a row and the number of rows of the reaction wells 4 according to the desired type of analysis.
  • the structure and capacity of the device for multi-channel electrochemical measuring of the invention is defined in particular by the number of the reaction wells 4 in each row of the reaction wells 4 and the corresponding number of the electrode systems 5 I connectors 9 on the lid 2 of the device.
  • the appropriate distance of the electrode systems 5 from the free edge of the lid 2 may also vary.
  • the cavity In addition to the sliding of the plate 3 in and out of the bottom portion 1 through the opening in the wall of the bottom portion 1_, it is possible to design the cavity without the opening in the wall of the bottom portion 1_, wherein the size of the cavity for inserting the plate 3 must be such as to allow movement of the plate 3 in a direction perpendicular to the row of the electrode systems 5.
  • the cavity must also include an element for preventing the movement of the plate 3 in a direction parallel to the row of the electrode systems 5.
  • FIG. 4a-4c An alternative embodiment of the carriers 8 of the electrode systems 5 is shown in fig. 4a-4c.
  • Fig. 4a shows a possible embodiment of the carrier 8 of the electrode systems 5, wherein each electrode system 5 has its own carrier 8 of the electrode systems 5.
  • Fig. 4b shows a group arrangement of 4 electrode systems 5 on one carrier 8 of the electrode systems 5.
  • Fig. 4c shows an embodiment of a single carrier 8 of the electrode systems 5 for all 8 electrode systems 5 (all electrode systems 5 of the exemplary embodiment of the invention are placed on one carrier 8 of the electrode systems 5 connected to one connector 9).
  • the number of the electrode systems 5 on the carrier 8 of the electrode systems 5 is not given, the maximum number of the electrode systems 5 on one carrier 8 of the electrode systems 5 is limited only by the number of all positions forming the row of the connectors 9 along the width of the free edge of the lid 2 of the device (e.g., in embodiments of the device with row of 12 connectors 9, the maximum number is 12 electrode systems 5 on one carrier 8 of the electrode systems 5).
  • the capillaries 10 for supplying the auxiliary medium may also be adapted to supply liquids to the reaction wells 4 or to drain liquids from the reaction wells 4. In the latter case, it is necessary to ensure that the mouth of the capillary 10 for supplying the auxiliary medium reaches the bottom of the reaction well 4 and allows the reaction well 4 to be completely emptied.
  • the device for multi-channel electrochemical measuring and alternative embodiments thereof according to the invention can be used for rapid electrochemical analysis of various samples within a single slidably movable plate 3 with a plurality of rows of reaction wells 4, which consists of successively immersing a row of electrode systems 5 into a respective row of reaction wells 4 on the plate 3.
  • the use of the device of the invention allows semi-automation and saving of time and handling steps when performing electrochemical analyses using a wide range of methods (e.g., voltammetric or amperometric analysis).
  • the device can be used in environmental, industrial, and clinical laboratories for identification and quantification of various substances such as heavy metals, organic pollutants, pharmaceuticals, markers in clinical samples, etc.
  • the above-described device for multi-channel electrochemical measuring and method of use thereof can be used in further analytical methods using electrode systems for measuring different samples or a combination of different procedures within one multiwell plate.

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Abstract

The object of the invention is a device for multi-channel electrochemical measuring and a method of use thereof. The device of the invention comprises a bottom portion (1), a lid (2), and a plate (3) comprising a plurality of reaction wells (4), wherein the lid (2) comprises a plurality of electrode systems (5), the bottom portion (1) is movably connected to the lid (2) and comprises a cavity for receiving the plate (3). All electrode systems (5) are arranged in at least one row of electrode systems (5), and the reaction wells (4) are arranged in parallel rows of the reaction wells (4), wherein each row of the reaction wells (4) comprises a number of the reaction wells (4) corresponding to the number of the electrode systems (5) in at least one row of the electrode systems (5), and the number of rows of the reaction wells (4) is greater than the number of rows of the electrode systems (5), wherein in the second position of the lid (2), the rows of the electrode systems (5) are parallel to the rows of the reaction wells (4) and the plate (3) is slidably movably connected to the bottom portion (1) in a direction perpendicular to the at least one row of the electrode systems (5).

Description

Device for multi-channel electrochemical measuring and method of use thereof
Technical Field
The invention relates to a device for multi-channel electrochemical measuring for performing a variety of electrochemical measurements within one plate comprising a plurality of reaction wells.
Background of the Invention
Previously known procedures for multi-channel electrochemical measurements of liquid samples use relatively large volumes of the examined sample in a flow-through arrangement (i.e. , more than 1 mL) or in a small volume (5.0 to 200 pL). One example is the use of a standard 96-well microtiter plate and an integrated layered electrode. However, such solution limits its application to only one use or one type of analysis in all reaction wells. When solutions need to be changed to modify or chemically alter the integrated layered electrodes, the solutions need to be added or aspirated by manual pipetting and electrodes and wells need to be rinsed, which increases the overall experimental time and the risk of unintentional contamination.
Another known arrangement uses multi-channel layered multi-electrodes, which are characterised by an arrangement of working electrodes in close proximity to the reference and auxiliary electrodes (i.e., all working electrodes share the auxiliary and reference electrodes). However, this solution also allows measurements in only one solution and does not allow simultaneous measurement of multiple samples.
Another known approach is the use of a multi-channel layered multi-electrode, characterised by arrangement of working electrodes on one undivided and unshaped carrier, where each working electrode has its own auxiliary and reference electrode. In this case, however, it is not possible to use such layered electrode assembly for measurements in a 96-well microtiter plate.
A disadvantage of the above solutions is the need for large amount of the analysed sample, complex design of the device, and large number of the electrode systems, which corresponds to the number of wells of the microtiter plate with the samples. For different types of measurements within one microtiter plate, manual pipetting and other steps are often required, which greatly complicate the electrochemical measurements and increase the risk of human error. Another disadvantage is that they do not allow measurements without the presence of oxygen in the measured solution.
Summary of the Invention
The above shortcomings are eliminated to a certain extent by a device for multichannel electrochemical measuring of the present invention. The device for multi-channel electrochemical measuring comprises a bottom portion, a lid, and a plate comprising a plurality of reaction wells for measured samples, wherein the lid comprises a plurality of the electrode systems. The bottom portion of the device is movably connected to the lid and comprises a cavity for receiving the plate, wherein the lid has a first position, in which all electrode systems are located outside the reaction wells, and a second position, in which all electrode systems are located at least partially inside the reaction wells. The electrode systems on the lid are arranged in at least one row of the electrode systems, and the reaction wells are arranged in parallel rows of the reaction wells, wherein each row of the reaction wells comprises a number of reaction wells corresponding to the number of the electrode systems in the at least one row of the electrode systems, and the number of rows of the reaction wells is greater than the number of rows of the electrode systems. In the second lid position, the rows of the electrode systems are parallel to the rows of the reaction wells, and the plate is slidably movably connected to the bottom portion in a direction perpendicular to the at least one row of the electrode systems. An advantage of the device of the invention lies in particular in the combination of the adjustable sliding movement of the plate with a plurality of reaction wells and the specific arrangement of the electrode systems, which allows the use of a single row of the electrode systems for different electrochemical measurements in rows of reaction wells within one plate, or alternatively, a row of the wells can be used to wash the electrode systems or to modify their surface.
In a preferred embodiment, the lid comprises just one row of the electrode systems placed on the underside of the lid along the edge of the lid from the underside of the lid. Placing the electrode systems in only one row saves electrode systems, wherein measurements in all rows of the reaction wells on the plate are made with one row of the electrode systems.
In a preferred embodiment, the lid is rotatably movably connected to the bottom portion by its first end and comprises a row of the electrode systems at its second end along the free edge of the lid, wherein the first end of the lid and the second end of the lid are located on the opposite sides of the lid. The advantage of this arrangement is that when the lid is closed, all electrode systems of the row of the electrode systems are simultaneously and equally immersed in the reaction wells.
The plate comprising a plurality of the reaction wells preferably comprises at least 6 rows of the reaction wells, and each row comprises at least 8 reaction wells, wherein the number of rows of the reaction wells is at least twice the number of rows of the electrode systems.
In a preferred embodiment, the bottom portion of the device of the invention comprises a stop for fixing the position of the plate. The stop is adjustable and serves for securing the plate such that when the lid of the electrode system is in the second position, it is at least partially inside the reaction wells of the respective row of the reaction wells on the plate.
The device for multi-channel electrochemical measuring further preferably comprises arresting of the lid. Using the height-adjustable lid, the depth of immersion of the electrode systems into the reaction wells on the plate can be regulated, or the analysis can be performed only on a drop of the measured sample. The arresting of the lid then ensures that the lid is fixed in position. The electrode systems are removably connected to the lid, wherein the electrode systems comprise a carrier and the lid comprises connectors adapted to removably connect the carrier of the electrode systems, wherein at least 2 electrode systems in one row of the electrode systems share a common carrier. An advantage of grouping the electrode systems in pairs or groups on one carrier is easier and faster exchange of the electrode systems/carriers from the connectors.
In a preferred embodiment, the lid comprises a plurality of capillaries for supplying an auxiliary medium to the electrode systems in the vicinity of the electrode systems, wherein each capillary is in the second position of the lid located at least partially within a reaction well in which the electrode system is also at least partially located. The capillaries for supplying the auxiliary medium can be used, for example, to saturate or bubble the sample in the reaction wells with auxiliary gas before or during the electrochemical measurement. This also enables performing electrochemical measurements without the presence of oxygen on the electrode system.
A preferred method of using the device for multi-channel electrochemical measuring comprises the following steps: when the lid is opened, the plate is inserted into the cavity for receiving the plate, and then the lid is closed, thereby bringing the first row of the electrode systems into a position where all the electrode systems of the first row of the electrode systems are at least partially located within the reaction wells of the first row of the reaction wells. When the lid is reopened, the first row of the electrode systems is brought to a position where all the electrode systems of the first row of the electrode systems are outside the reaction wells and subsequently the plate is displaced relative to the bottom portion perpendicular to the first row of the electrode systems, wherein after the lid is subsequently closed, the first row of the electrode systems is brought into a position where all the electrode systems of the first row of the electrode systems are at least partially located inside the reaction wells of the second row of the reaction wells, wherein the plate comprises both the first row of the reaction wells and the second row of the reaction wells. Description of Drawings
A summary of the invention is further described by means of exemplary embodiments thereof, which are described with reference to the accompanying drawings, in which: fig. 1 shows a section through the device for multi-channel electrochemical measuring of the invention with the lid placed in the second position, fig. 2 shows a front view of the device for multi-channel electrochemical measuring of the invention with the lid placed in the first position, fig. 3 shows a section through the electrode system when immersed in the reaction well, fig. 4a shows an embodiment of one carrier for one electrode system, fig. 4b shows an embodiment of one carrier for 4 electrode systems, and fig. 4c shows an embodiment of one carrier for 8 electrode systems.
Exemplary Embodiments of the Invention
The invention will be further described using exemplary embodiments with reference to the respective drawings. One exemplary embodiment is a structure of the device for multi-channel electrochemical measuring of the invention shown in figs. 1 and 2.
The structure of the device for multi-channel electrochemical measuring of the exemplary embodiment comprises a bottom portion 1_, a lid 2, and a plate 3 comprising a plurality of reaction wells 4, wherein the lid 2 comprises precisely one row of the electrode systems 5. The bottom portion 1. has the shape of a plate, wherein the bottom portion 1. comprises a cavity adapted for inserting the plate 3 with a plurality of the reaction wells 4 which opens on the top side of the bottom portion 1_. The plate 3 with plurality of the reaction wells 4 is, in this exemplary embodiment, a standard microtiter plate with 96 reaction wells 4 comprising 12 rows of the reaction wells 4, wherein each row of the reaction wells 4 comprises 8 reaction wells 4. The plate 3 is slidably movably disposed on the bottom portion 1_ and slidable in the plane of the upper surface of the bottom portion 1. in a direction perpendicular to the row of the electrode systems 5 attached to the lid 2. Thus, the plate 3 has a first position where all electrode systems 5 of the row of the electrode systems 5 are at least partially located inside the reaction wells 4 of the first (outermost) row of the reaction wells 4, and a second position where all electrode systems 5 of the row of the electrode systems 5 are located at least partially inside the reaction wells 4 of the second row of the reaction wells 4 of the plate 3. The bottom portion 1_ comprises a passageway in the wall opening into the cavity through which the plate 3 can be slid in and out, wherein the cavity comprises guide grooves enabling movement of the plate 3 in a direction perpendicular to the row of the electrode systems 5 while preventing movement of the plate 3 in a direction parallel to the row of the electrode systems 5. The bottom portion 1. of the device further comprises an adjustable stop 6 for fixing the position of the plate 3.
The lid 2 in the first exemplary embodiment has the shape of a plate rotatably movably connected to the bottom portion 1_, wherein the connection of the lid 2 to the bottom portion 1. is located at the first end of the lid 2. At the other end of the lid 2 along the free edge, the lid 2 comprises a row of the electrode systems 5, wherein the first end of the lid 2 and the second end of the lid 2 are located on opposite sides of the lid 2. In the first exemplary embodiment, the lid 2 comprises electrode systems 5 arranged in precisely one row of the electrode systems 5, wherein the row of the electrode systems 5 is placed on the underside of the lid 2 along the free edge of the lid 2 at a distance of 2 to 10 mm, preferably 3 to 6 mm from the margin of the free edge of the lid 2. The lid 2 has a first position in which all electrode systems 5 of the row of the electrode systems 5 are located outside the reaction wells 4 of the plate 3 (view of the device of fig. 2), and a second position in which all electrode systems 5 of the row of the electrode systems 5 are located at least partially inside the reaction wells 4 belonging to the first (outermost) row of the reaction wells 4 of the plate 3 (section through the device of fig. 1 ). The direction of the movement of the lid 2 during opening is shown by the corresponding arrow in fig. 1 . The definition of the sliding movement of the plate 3 in the direction perpendicular to the row of the electrode systems 5 relates to the placement of the lid 2 in the second position. The lid 2 of the device for multi-channel electrochemical measuring comprises, on the side adjacent to the bottom portion 1_, a plurality of connectors 9 placed in a row along the free edge of the lid 2, adapted for connecting and securing the carriers 8 of the electrode systems 5. In this exemplary embodiment, the electrode systems 5 are layered electrode systems. This exemplary embodiment of the device of the invention comprises a total of 8 connectors 9, where the carrier 8 of the electrode systems 5 with one or more electrode systems 5 may be connected to each connector 9. Possible arrangements of the electrode systems 5 on the carrier 8 of the electrode systems 5 will be further described in alternative embodiments according to the present invention with reference to figs. 4a-4c. All connectors 9 for the carriers 8 of the electrode systems 5 are connected through an electric line to the output connector 11 connecting the device for multi-channel electrochemical measuring of the present invention with a measuring device, e.g., a multichannel potentiostat.
In a first exemplary embodiment of the device of the present invention, capillaries 10 for supplying the auxiliary medium from the auxiliary medium source 12 are placed on the lid 2 in a row in front of or behind the connectors 9 or the carriers 8 of the electrode systems 2. The auxiliary medium source 12 is, in the first exemplary embodiment, any auxiliary or inert gas, e.g., nitrogen or argon. The capillary 10 for supplying the auxiliary medium has a tapered mouth directed towards the surface of the electrode system 5 and allows saturation or bubbling of the analysed sample in the reaction well 4 with the selected gas or removal of oxygen from the analysed sample before or during the electrochemical measurement. In the second position of the lid 2, the capillaries 10 for the auxiliary medium are located at least partially inside the reaction wells 4.
With the lid 2 in the second position, the electrode systems 5 are at least partially immersed in the respective reaction wells 4, this detail is shown in fig. 3. The depth of immersion of the electrode systems 5 into the reaction wells 4 is regulated by movement of the lid 2. In this exemplary embodiment, the lid 2 is rotatably movably connected to the bottom portion 1_, wherein the vertical position of the electrode systems 5 can be adjusted by moving the lid 2, and the position of the lid 2 can be arrested using an arresting screw placed on the pivot pin of the lid 2. By adjusting the arresting 7, electrochemical measurements can be made also for samples with extremely small volumes or in a single drop (at least 3 pL) of the analysed sample applied on each carrier 8 of the electrode system 5 at the location of the electrode system 5. The method of use of the device for multi-channel electrochemical measuring of an exemplary embodiment comprises the following consecutive steps:
1 . opening the lid 2 (the lid 2 is in the first position),
2. inserting the plate 3 into the cavity for receiving the plate 3 in the bottom portion 1_,
3. closing the lid 2 (the plate 3 is in the first position and the lid 2 is in the second position, wherein all electrode systems 5 of the first row of the electrode systems 5 are at least partially located inside the reaction wells 4 of the first (outermost) row of the reaction wells 4),
4. starting the electrochemical measurement,
5. termination of the electrochemical measurement,
6. opening the lid 2 (the lid 2 is in the first position),
7. displacement of the plate 3 in the plane of the plate 3 in a direction perpendicular to the row of the electrode systems 5,
8. closing the lid 2 (the plate 3 is in the second position and the lid 3 is in the second position, wherein all electrode systems 5 of the first row of the electrode systems 5 are at least partially located inside the reaction wells 4 of the second row of the reaction wells 4),
9. repeating steps 4 to 8, wherein when closing the lid 2, the lid 2 is in the second position and all electrode systems 5 of the first row of the electrode systems 5 are at least partially located inside the reaction wells 4 of the third to twelfth row of the reaction wells 4.
Alternatively, other operations besides the electrochemical measurement itself may be performed in steps 5 and 6 according to the above method of use of the device. The analysed sample or an auxiliary substance, e.g., a cleaning solution, may be placed in the entire selected rows of wells 4, wherein the row of wells 4 may be used, e.g., for rinsing the electrode systems 5, modifying the electrode systems 5, or for interaction studies. If necessary, the above steps may include the steps of fixing the position of the plate 3 by means of the stop 6 or readjusting the position of the lid 2 and its subsequent arresting 7.
The method of use of the device of the first exemplary embodiment of the invention preferably enables saturation or bubbling of the analysed sample in the reaction well 4 with a selected auxiliary gas (e.g., nitrogen, argon) or removing oxygen from the analysed sample before or during the electrochemical measurement. The gas supply from the auxiliary medium source 12 to the capillaries 10 for supplying the auxiliary medium can be opened and closed before or at any time during the electrochemical measurement.
In the following section, alternatives in embodiments of elements of the device for multi-channel electrochemical measuring of the invention will be described.
In an alternative embodiment of the device of the invention, the lid 2 may comprise multiple rows of the electrode systems 5, e.g., precisely two parallel rows of the electrode systems 5. The first row of the electrode systems 5 is positioned on the underside of the lid 2 along the free edge of the second end of the lid 2 as in the first exemplary embodiment of the device of the invention, wherein the second row of the electrode systems 5 is positioned on the underside of the lid 2 parallel to the first row of the electrode systems 5. The plate 3 in this embodiment is also a 96-well microtiter plate. The gap, or distance, between the first row of the electrode systems 5 and the second row of the electrode systems 5 corresponds to a multiple of the width of one row of the reaction wells 4, wherein in this embodiment, this gap between the rows of the electrode systems 5 corresponds to a multiple of 5 times the width of the row of the reaction wells 4, wherein, in the first position of the plate 3 and the second position of the lid 2, the first row of the electrode systems 5 is at least partially located inside the first (outermost) row of the reaction wells 4 and, at the same time, the second row of the electrode systems 5 is at least partially located inside the seventh row of the reaction wells 4 on the plate 3. In the second position of the plate 3 and the second position of the lid 2, the first row of the electrode systems 5 is located at least partially inside the second row of the reaction wells 4, and at the same time, the second row of the electrode systems 5 is at least partially inside the eighth row of the reaction wells 4 on the plate 3. Thus, the first row of the electrode systems 5 may be located at least partially inside the first (outermost) to sixth row of the reaction wells 4 during the measurement throughout the entire plate 3, and the second row of the electrode systems 5 may be located continuously at least partially inside the seventh to twelfth row of the reaction wells 4. Electrochemical measurement, optionally rinsing, and other procedures can thus be carried out in two rows of the reaction wells 4 simultaneously. Some rows of the reaction wells can be used to clean or modify the electrode surface.
Another possible embodiment of the device of the invention comprises the same method of movably connecting the lid 2 to the bottom portion 1. as in the first exemplary embodiment, differing only in the position of the rotatable connection of the lid 2 to the bottom portion 1_. In further embodiments, the rotatable connection of the lid 2 to the bottom portion 1. may be located at any lateral edge of the lid 2 between the first end and the second end of the lid 2, wherein the axis of rotation of the rotatable connection is parallel to the direction of movement of the plate 3. However, the rows of the electrode systems 5 must still be oriented perpendicularly to the movement of the plate 3 in the second position of the lid 2.
Alternative embodiments of the device of the invention may include other options of movable connection and mutual orientation of the bottom portion 1_ and the lid 2. Any suitable mechanical, hydraulic, pneumatic, or combined lifting system, e.g., parallelogram, screwjack, scissor jack, piston jack, etc., can be used to height-adjust and move the lid 2.
Other possible embodiments of the invention may include various types of plates 3 having a plurality of the reaction wells 4 varying in the number of the reaction wells 4 in a row and the number of rows of the reaction wells 4 according to the desired type of analysis. Thus, the structure and capacity of the device for multi-channel electrochemical measuring of the invention is defined in particular by the number of the reaction wells 4 in each row of the reaction wells 4 and the corresponding number of the electrode systems 5 I connectors 9 on the lid 2 of the device. Depending on the dimensions of the particular plate 3, the appropriate distance of the electrode systems 5 from the free edge of the lid 2 may also vary. In addition to the sliding of the plate 3 in and out of the bottom portion 1 through the opening in the wall of the bottom portion 1_, it is possible to design the cavity without the opening in the wall of the bottom portion 1_, wherein the size of the cavity for inserting the plate 3 must be such as to allow movement of the plate 3 in a direction perpendicular to the row of the electrode systems 5. The cavity must also include an element for preventing the movement of the plate 3 in a direction parallel to the row of the electrode systems 5.
An alternative embodiment of the carriers 8 of the electrode systems 5 is shown in fig. 4a-4c. Fig. 4a shows a possible embodiment of the carrier 8 of the electrode systems 5, wherein each electrode system 5 has its own carrier 8 of the electrode systems 5. Fig. 4b shows a group arrangement of 4 electrode systems 5 on one carrier 8 of the electrode systems 5. Fig. 4c shows an embodiment of a single carrier 8 of the electrode systems 5 for all 8 electrode systems 5 (all electrode systems 5 of the exemplary embodiment of the invention are placed on one carrier 8 of the electrode systems 5 connected to one connector 9). In alternative embodiments of the invention, the number of the electrode systems 5 on the carrier 8 of the electrode systems 5 is not given, the maximum number of the electrode systems 5 on one carrier 8 of the electrode systems 5 is limited only by the number of all positions forming the row of the connectors 9 along the width of the free edge of the lid 2 of the device (e.g., in embodiments of the device with row of 12 connectors 9, the maximum number is 12 electrode systems 5 on one carrier 8 of the electrode systems 5).
In alternative embodiments of the device of the invention, the capillaries 10 for supplying the auxiliary medium may also be adapted to supply liquids to the reaction wells 4 or to drain liquids from the reaction wells 4. In the latter case, it is necessary to ensure that the mouth of the capillary 10 for supplying the auxiliary medium reaches the bottom of the reaction well 4 and allows the reaction well 4 to be completely emptied.
The device for multi-channel electrochemical measuring and alternative embodiments thereof according to the invention can be used for rapid electrochemical analysis of various samples within a single slidably movable plate 3 with a plurality of rows of reaction wells 4, which consists of successively immersing a row of electrode systems 5 into a respective row of reaction wells 4 on the plate 3. The use of the device of the invention allows semi-automation and saving of time and handling steps when performing electrochemical analyses using a wide range of methods (e.g., voltammetric or amperometric analysis). The device can be used in environmental, industrial, and clinical laboratories for identification and quantification of various substances such as heavy metals, organic pollutants, pharmaceuticals, markers in clinical samples, etc.
Industrial Applicability
The above-described device for multi-channel electrochemical measuring and method of use thereof can be used in further analytical methods using electrode systems for measuring different samples or a combination of different procedures within one multiwell plate.
List of Reference Numbers
1 - bottom portion
2 - lid
3 - plate 4 - reaction well
5 - electrode system
6 - stop
7 - arresting
8 - carrier
9 - connector
10 - capillary for supplying the auxiliary medium
11 - output connector
12 - auxiliary medium source

Claims

1 . A device for multi-channel electrochemical measuring comprising a bottom portion (1 ), a lid (2), and a plate (3) comprising a plurality of reaction wells (4), wherein the lid (2) comprises a plurality of electrode systems (5), the bottom portion (1 ) is movably connected to the lid (2) and comprises a cavity for receiving the plate (3), wherein the lid (2) has a first position in which all electrode systems (5) are located outside the reaction wells (4), and a second position in which all electrode systems (5) are located at least partially inside the reaction wells (4), characterised in that all electrode systems (5) are arranged in at least one row of the electrode systems (5) and the reaction wells (4) are arranged in parallel rows of the reaction wells (4), wherein each row of the reaction wells (4) comprises a number of the reaction wells (4) corresponding to the number of the electrode systems (5) in at least one row of the electrode systems (5) and the number of rows of the reaction wells (4) is greater than the number of rows of the electrode systems (5), wherein, in the second position of the lid (2), the rows of the electrode systems (5) are parallel to the rows of the reaction wells (4) and the plate (3) is slidably movably connected to the bottom portion (1 ) in a direction perpendicular to the at least one row of the electrode systems (5).
2. The device for multi-channel electrochemical measuring of claim 1 , characterised in that the lid (2) comprises precisely one row of the electrode systems (5), wherein this row is located along the edge of the lid (2) from the underside of the lid (2).
3. The device for multi-channel electrochemical measuring of claims 1 to 2, characterised in that the lid (2) is rotatably movably connected by its first end to the bottom portion (1 ) and at its second end along the free edge of the lid (2) it comprises a row of the electrode systems (5), wherein the first end of the lid (2) and the second end of the lid (2) are located on opposite sides of the lid (2).
4. The device for multi-channel electrochemical measuring of claims 1 to 3, characterised in that the plate (3) comprises at least 6 rows of the reaction wells (4), and each row comprises at least 8 reaction wells (4), wherein the number of rows of the reaction wells (4) is at least twice the number of rows of the electrode systems (5).
5. The device for multi-channel electrochemical measuring of claims 1 to 4, characterised in that the bottom portion (1 ) comprises a stop (6) for fixing the position of the plate (3).
6. The device for multi-channel electrochemical measuring of claims 1 to 5, characterised in that it comprises arresting (7) of the lid (2).
7. The device for multi-channel electrochemical measuring of claims 1 to 6, characterised in that the electrode systems (5) are removably connected to the lid (2), wherein the electrode systems (5) comprise a carrier (8) and the lid (2) comprises connectors (9) adapted to removably connect the carrier (8), wherein at least 2 electrode systems (5) within one row of the electrode systems (5) share a common carrier (8).
8. The device for multi-channel electrochemical measuring of claims 1 to 7, characterised in that the lid (2) comprises a plurality of capillaries (10) for supplying an auxiliary medium to the electrode systems (5) in the vicinity of the electrode systems (5), wherein each capillary (10) is in the second position of the lid (2) located at least partially inside the reaction well (4) in which the electrode system (5) is also at least partially located.
9. A method of use of the device for multi-channel electrochemical measuring of claims 1 to 8, wherein: when the lid (2) is open, the plate (3) is inserted into a cavity for receiving the plate (3) and subsequently the lid (2) is closed, thereby bringing the first row of the electrode systems (5) into a position where all electrode systems (5) of the first row of the electrode systems (5) are at least partially located inside the reaction wells (4) of the first row of reaction wells (4), further, when the lid (2) is reopened, the first row of the electrode systems (5) is brought to a position where all electrode systems (5) of the first row of the electrode systems (5) are located outside the reaction wells (4), characterised in that the plate (3) is subsequently displaced relative to the bottom portion (1 ) perpendicular to the first row of the electrode systems (5), wherein after subsequent closing of the lid (2), the first row of the electrode systems (5) is brought to a position where all electrode systems 16
(5) of the first row of the electrode systems (5) are at least partially located inside the reaction wells (4) of the second row of the reaction wells (4), wherein the plate (3) comprises both the first row of the reaction wells (4) and the second row of the reaction wells (4).
10. The method of use of the device for multi-channel electrochemical measuring of claim 9, characterised in that after displacing the plate (3), the position of the plate (3) is arrested by the stop (6).
11. The method of use of the device for multi-channel electrochemical measuring of claims 9 and 10, characterised in that after closing the lid (2), the analysed sample in the reaction well (4) is saturated or bubbled with an auxiliary gas by means of capillaries (10) for supplying the auxiliary medium.
PCT/CZ2021/050119 2021-10-29 2021-10-29 Device for multi-channel electrochemical measuring and method of use thereof WO2023072317A1 (en)

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Citations (3)

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US6247350B1 (en) * 1997-04-24 2001-06-19 Daikin Industries Limited Sensor
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Title
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