WO2007097246A1 - Test sample preparation device - Google Patents

Test sample preparation device Download PDF

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Publication number
WO2007097246A1
WO2007097246A1 PCT/JP2007/052801 JP2007052801W WO2007097246A1 WO 2007097246 A1 WO2007097246 A1 WO 2007097246A1 JP 2007052801 W JP2007052801 W JP 2007052801W WO 2007097246 A1 WO2007097246 A1 WO 2007097246A1
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WO
WIPO (PCT)
Prior art keywords
separation
test sample
communication
extraction
liquid
Prior art date
Application number
PCT/JP2007/052801
Other languages
French (fr)
Japanese (ja)
Inventor
Masayoshi Momiyama
Seiko Watanabe
Atsushi Hattori
Masato Kon
Original Assignee
Aisin Seiki Kabushiki Kaisha
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
Application filed by Aisin Seiki Kabushiki Kaisha filed Critical Aisin Seiki Kabushiki Kaisha
Publication of WO2007097246A1 publication Critical patent/WO2007097246A1/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/56Labware specially adapted for transferring fluids
    • B01L3/563Joints or fittings ; Separable fluid transfer means to transfer fluids between at least two containers, e.g. connectors
    • B01L3/5635Joints or fittings ; Separable fluid transfer means to transfer fluids between at least two containers, e.g. connectors connecting two containers face to face, e.g. comprising a filter
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/06Valves, specific forms thereof
    • B01L2400/0633Valves, specific forms thereof with moving parts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/06Valves, specific forms thereof
    • B01L2400/0633Valves, specific forms thereof with moving parts
    • B01L2400/0644Valves, specific forms thereof with moving parts rotary valves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01LCHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00Moving or stopping fluids
    • B01L2400/06Valves, specific forms thereof
    • B01L2400/0633Valves, specific forms thereof with moving parts
    • B01L2400/065Valves, specific forms thereof with moving parts sliding valves

Definitions

  • the present invention relates to a test sample preparation apparatus for separating and extracting a test substance from a test sample.
  • instrumental analysis based on the measurement principle such as chromatography or mass spectrometry is the mainstream for determining the presence or absence of a specific substance and its content.
  • the measurement target substance contained in the analysis sample containing various substances such as river water, soil, food, etc. is preferentially extracted from the analysis sample before the analysis.
  • the mainstream is to perform a process called pretreatment for purification.
  • pretreatments a combination of various operations such as dissolution of analysis sample, liquid-liquid extraction, solid-liquid extraction, centrifugation, gel electrophoresis, distillation, column chromatography, and concentration by evaporation of solvent is combined. There are many.
  • the pretreatment for extracting and purifying the measurement substance from the analytical sample is an important task that is highly necessary for various analytical methods.
  • the pretreatment of extracting and purifying the measurement substance from the analytical sample is an important task that is highly necessary in various analytical methods.
  • These pretreatments can be a combination of a number of different operations such as sample dissolution, liquid-liquid extraction, solid-liquid extraction, centrifugation, gel electrophoresis, distillation, column chromatography, and solvent evaporation.
  • sample dissolution liquid-liquid extraction
  • solid-liquid extraction centrifugation
  • gel electrophoresis gel electrophoresis
  • distillation column chromatography
  • solvent evaporation solvent evaporation.
  • This is only an example, but taking liquid-liquid extraction using a widely used separatory funnel as an example, after mixing two liquids, visually check the interface between the two separated liquids, Only one solution is manually collected in an Erlenmeyer flask. Separation funnels are glass devices that are simply covered with a lid, and the operator is likely to be exposed to chemicals due to liquid leakage during operation.
  • the pretreatment method varies depending on the sample to be analyzed and the substance to be measured. For this reason, there are many cases where it is difficult to use an automatic analyzer because it is difficult to make a routine work, and it is easy to cause human error. It has become a problem.
  • the pretreatment step is “silica gel column. Purification and liquid extraction using a separatory funnel are often used, and these processes require a high level of expertise in the workers such as dexterity, agility, visual acuity, and judgment. As a result, the measurement results vary, which hinders the spread of analysis.
  • the present invention has been completed in view of the above circumstances, and solves the problem of providing a test sample preparation apparatus that can easily perform pretreatment in a sealed state in an analysis method that requires complicated pretreatment. It should be a challenge.
  • the test sample preparation apparatus of the present invention that solves the above problems is selected from dissolution, liquid-liquid extraction, solid-liquid extraction, filtration, liquid separation, adsorption, and reaction for a solid or liquid test sample. It is a test sample preparation device that separates and extracts a test substance through one or more separation and extraction processes. In carrying out these separation and extraction steps, the number of unit containers required for one or more separation and purification steps is used, and the test samples are sequentially transferred between the unit vessels. In other words, the test sample is pretreated by moving sequentially between unit containers.
  • the unit container can have a separation and extraction member corresponding to the separation and extraction step to be performed in the internal space, and an efficient separation and extraction step can be realized.
  • the unit container includes a container body part and a communication path forming member
  • the container main body has an internal space partitioned to accommodate the test sample, and the communication path forming member is connected to the container main body and sealed to the communication path forming member provided in another unit container. It is possible to switch between a connection state and a shut-off state between a connectable connection portion and an internal space of the container main body portion connected to the internal space of the container main body portion connected in a sealed state.
  • the two unit containers are connected in a sealed state, and then the inside is communicated.
  • various members for example, a solvent for dissolution / extraction
  • the unit containers to be combined may be the same, and at least a part of the plurality of unit containers may have a different structure from the remaining unit containers. Whether to adopt the same or different ones can be selected appropriately according to the separation and extraction process. '
  • the unit container other parts (for example, the shape of the container body part) can be used if connection can be realized between the communication path forming members of the unit container that is actually connected when the test sample and separation / extraction member are moved sequentially.
  • ⁇ Size Type of separation / extraction member arranged inside, structure of communication path forming member (thing that can be connected to each other but not the same structure) 'size' is not particularly limited.
  • an air valve connected to the container body or the communication path forming member and communicating with the outside may be provided.
  • the container body portion is desirable because it has an uneven portion on the inner wall, so that an improvement in the stirring effect can be expected.
  • the separation and extraction member when the separation and extraction step is a dissolution step, a solution is exemplified.
  • the said separation and extraction process when the said separation and extraction process is a filtration process, the said separation and extraction member can illustrate a filtration member.
  • the separation and extraction step is a liquid separation step
  • the separation and extraction member includes a tubular member located in the vicinity of the interface between the two liquids separated by the tip, and the upper layer portion of the test sample is sucked from the tubular member And a suction means.
  • the separation and extraction member has one lower layer of two liquids to be separated.
  • An example is a tubular member having a tip located on the liquid level when moved from one container to the other and having a cock inside.
  • the separation and extraction member when the separation and extraction step is a liquid separation step, the separation and extraction member performs selective filtration using a difference in the degree of hydrophilicity and Z or lipophilicity of two liquids to be separated. Examples are filtration members with controlled surface hydrophilicity and Z or lipophilicity. Further, the separation and extraction member in the case where the separation and extraction step is an adsorption step is exemplified by an adsorption member. Specific examples of a set of communication path forming members that can be connected to each other are as follows:
  • a cylindrical member having a cylindrical member communication hole provided eccentrically on the end surface, and a rotating member communication hole having substantially the same shape as the end surface of the cylindrical member and having the same degree of eccentricity.
  • a rotating member disposed in close contact with the end surface and rotatably disposed between a position where the cylindrical member communicating hole and the rotating member communicating hole coincide with a position shifted from each other.
  • One of the communication path forming members includes a cylindrical member having a cylindrical member communication hole provided on an end surface, a closing member capable of closing the cylindrical member communication hole, and connecting the blocking member from the inside of the cylindrical member to the cylindrical member communication Biasing means for biasing toward the hole,
  • the other communication path forming member is a member provided with closing member moving means for moving the closing member of one communication path forming member into the cylindrical member when connected to the one communication path forming member.
  • One set of the communication path forming members connected to each other includes two end surface members having end surface member communication holes provided on opposite end surfaces, and the end surface members between the end surface members.
  • a communication switching member provided movably along the end surface and having a communication hole communicating between the end surface member communication holes of the two end surface members; and following the movement of the communication switching member
  • a thin-film sealing member that closes and closes the end surface member communication hole when the communication switching member is pulled out from between the two end surface members.
  • FIG. 1 is a schematic explanatory diagram of a first embodiment of a test sample preparation apparatus according to the present invention.
  • FIG. 2 is a schematic diagram for explaining the operation of the apparatus of FIG.
  • FIG. 3 is a schematic explanatory diagram of a second embodiment of the test sample preparation apparatus according to the present invention.
  • FIG. 4 is a schematic explanatory diagram of a third embodiment of the test sample preparation apparatus according to the present invention.
  • FIG. 5 is a schematic explanatory diagram of a fourth embodiment of the test sample preparation apparatus according to the present invention.
  • test sample preparation apparatus of the present invention will be described in detail below.
  • the test sample preparation apparatus of this embodiment is an apparatus used when a test substance contained in a test sample is separated and extracted in a plurality of steps. For example, it can be suitably used for pretreatment of test samples in the measurement of PCB contamination.
  • Test samples can be solid or liquid.
  • a suspension in which a solid is dispersed in a liquid can be targeted.
  • the pretreatment for the test sample can be applied to one or more processes selected from dissolution, liquid-liquid extraction, solid-liquid extraction, filtration, liquid separation, adsorption and reaction.
  • the pretreatment is the process of finally separating and extracting the test substance to be measured from the test sample, and at that time, impurities that affect the measurement are not mixed.
  • dissolution is a process in which a solid, suspension, slurry, or the like is dissolved in a solution to make a homogeneous solution.
  • Liquid-liquid extraction is a process in which a test substance is extracted with a liquid from a test sample dissolved in a liquid or solution. The target test substance can be separated by mixing the extract that is not mixed with the liquid test sample, transferring the test substance into the extract, and then separating the extract. Conversely, an extraction solution that dissolves only the impurities is used as a process for removing impurities from the test sample. You can also. Solid-liquid extraction can be used as a process for separating and removing impurities as well as separating and extracting test substances from solid test samples.
  • Filtration is a process of separating and removing solids that are impurities from a liquid or solution test sample and separating and extracting solids containing a test substance. Separation is a process that separates two unmixed solvents used in processes such as liquid-liquid extraction.
  • Adsorption is a process of adsorbing and removing impurities from a liquid test sample or separating and extracting a test substance by adsorption. When the test substance is separated and extracted by adsorption, the test substance is eluted with some extraction solvent (elution solvent) after adsorption.
  • the reaction should be performed only when a reaction reagent such as a liquid or solid is added to the test sample before pretreatment of the test sample. .
  • the separation and extraction process is a process that separates and extracts the test substance from the test sample by using one or a combination of two or more of these processes, and reduces the impurity content to the extent that it does not affect the analysis. .
  • This combination is not particularly limited because it varies greatly depending on the test substance. '
  • a plurality of unit containers are combined.
  • the plurality of unit containers used may be the same or different. Since the separation and extraction processes performed in each unit container are often considered to be different from each other, there may be cases where a plurality of unit containers are not all the same.
  • the unit container has a container main body, a communication path forming member, and other constituent elements as necessary.
  • the container body has an internal space partitioned to accommodate test samples and the like, and is a place where the separation and extraction process is performed.
  • the separation and extraction process can be performed by sequentially moving the test sample in a plurality of unit containers, and members used for separation and extraction between other unit containers and one unit container (separation extraction member) ) Can be completed in one unit container.
  • the unit container to which the test sample is moved after each process is applied is not particularly limited.
  • the inner wall of the container body can have an uneven portion for the purpose of improving the stirring effect.
  • air (vent) A valve, pressurizing means, or decompressing means may be connected.
  • the pressurizing means and the depressurizing means a combination of a cylindrical member and a piston moving inside the cylinder, or a rubber bag formed from an elastic body used for a syringe or the like can be used as in the case of a syringe.
  • a test sample introduction path which is an introduction path for introducing a test sample from the outside can be provided in the container body.
  • a test sample is a solid or liquid
  • a general lid or the like can be used.
  • the test sample is a liquid
  • a film made of an elastic material can be used.
  • the lid is opened to form an opening, and the test sample is introduced through the opening.
  • a 1 "biological membrane is a pathway through which a test sample is introduced into the inside using a syringe, etc.
  • the communication path forming member has a connection portion and a switching portion.
  • the connecting portion is a member that is connected to the container main body and can be connected in a sealed state to a communication path forming member provided in another unit container.
  • the switching part can be switched between a communication state and a shut-off state between the internal space of the container body part of the container and the internal space of the counterpart container body connected in a sealed state, and the test sample in the communication state. It is a member that can exchange.
  • the connecting portion is made at an opening provided in the container main body of each unit container. Make a sealed connection between these openings.
  • the switching unit is a means that can open and close this opening. Therefore, the connecting portion and the switching portion are highly related members, and their configurations are also closely related.
  • the first (second) unit container has a first (second) container body and a first (second) communication path forming member.
  • a structure including a cylindrical member and a rotating member As shown in FIG. 1, this structure is formed between the cylindrical member 10 of the first communication path forming member and the rotating member 11 1, and the cylinder of the second communication path forming member. Between the member 13 and the rotating member 12, each is rotatably arranged.
  • the cylindrical member 10 in the first communication path forming member has a cylindrical member communication hole 10 1 and a rotation restricting pin 10 2 protruding from the end surface on the end surface.
  • the cylindrical member communication hole 10 1 is formed eccentrically on the end face of the cylindrical member 10.
  • a rotating member 11 is rotatably provided on the end surface of the cylindrical member 10.
  • the rotating member 1 1 has a rotating member communication hole 1 1 1, a rotation restricting pin 1 1 2 protruding in the opposite direction of the cylindrical member 10, and a turn restricting groove 1 1 3.
  • the rotation restricting pin 10 0 2 of the cylindrical member 10 is inserted into the rotation restricting groove 1 1 3 of the rotating member 1 1, and as shown in FIG. 2 (a), (a-1) and (a — The range of rotation is restricted between 2).
  • the position of (a-1) is in a cut-off state because the cylindrical member communication hole 10 0 1 of the cylindrical member 10 and the rotating member communication hole 1 1 1 are displaced.
  • the position of (a-2) is rotated 90 ° counterclockwise from the position of (a-1), and the cylindrical member communication hole 1 0 1 and the rotation member communication hole 1 1 1 Are in communication with each other.
  • the cylindrical member 13 in the second communication path forming member has a cylindrical member communication hole 13 1 and a rotation restricting groove 13 2 formed on the end face.
  • a rotating member 12 is rotatably provided on the end surface of the cylindrical member 13.
  • the rotation member 1 2 has a rotation member communication hole 1 2 1, a rotation restricting pin 1 2 2 protruding to the cylindrical member 1 3 side, and a rotation restricting groove 1 2 3.
  • the rotation restricting pin 1 2 2 of the rotating member 1 2 is inserted into the rotation restricting groove 1 3 2 of the cylindrical member 1 3, and as shown in FIG. 2 (c), (c ⁇ l) and (c — The range of rotation is restricted between 2).
  • the position of (c 1 1) is in a blocked state because the cylindrical member communication hole 13 1 of the cylindrical member 13 is displaced from the rotating member communication hole 1 2 1.
  • the position of (c 1 2) is rotated 90 ° counterclockwise from the position of (c 1 1), and the cylindrical member communication hole 1 3 1 and the rotating member communication hole 1 2 1 Are in communication with each other.
  • the first container and the second container are connected by overlapping the rotating member 11 in the first communication path forming member and the rotating member 12 in the second communication path forming member.
  • the rotation restricting pin 1 1 2 in the rotating member 11 of the first communication path forming member is inserted into the rotation restricting groove 1 2 3 in the second communication path forming member.
  • (B-1) and (b-2) restrict the rotation range.
  • the position of (b-1) is in the blocked state because the rotation member communication hole 1 1 1 and the rotation member communication hole 1 2 1 are displaced. It is.
  • the position of (b-2) is rotated 90 ° counterclockwise from the position of (b-1), and the rotation member communication hole 1 1 1 and the rotation member communication hole 1 2 1 are the same. Then it is in communication.
  • the first communication path forming member of the first container and the second communication path forming member of the second container are connected, and then both are brought to the second state.
  • the first container and the second container are in communication with each other, and after exchanging the separation and extraction members necessary for the separation and extraction process, the first container is rotated to the opposite side. It becomes possible to turn it into a shut-off state again.
  • a wiper (not shown) can be provided on the end face of the cylindrical member or the surface of the rotating member to prevent contamination.
  • the wiper can be provided as a linear protrusion extending radially on each surface.
  • a cylindrical member communication hole 1 0 1 ′ is provided on the end face 10 ′ of the cylindrical member in the first communication path forming member, and further, a rotating member 1 1 provided with a rotating member communication hole 1 1 1 ′. It is the same as the above configuration in that 'is rotatably provided on its end face 10,.
  • the cylindrical member communication hole is also formed in the end surface 1 3 ′ of the cylindrical member in the second communication path forming member.
  • the positions of the rotating claws 1 1 4 and 1 2 4 provided on the rotating members 1 1 1 ′ and 1 2 ′ are also aligned.
  • the rotating claws 1 1 4 ′ and 1 2 4 ′ are rotated, and the cylindrical member communication holes 1 0 1 ′, the rotating member communication holes 1 1 1 ′,
  • the first container and the second container can be in communication.
  • the rotating claws 1 1 4 ′ and 1 2 4 ′ are used to rotate the rotating members 1 1 and 1 2, and the cylindrical member communicating holes 1 0 1 ′ and the rotating member communicating holes 1 1 1
  • the first container and the second container can be shut off.
  • FIG. 4 shows a state where the first container and the second container are combined.
  • the first container main body 20 and the second container main body 23 are arranged so that the end surface member 22 and the end surface member 25 are opposed to each other with a predetermined interval.
  • Each of the end surface members 2 2 and 25 has an end surface member communication hole, and the communication holes are closed by the closing members 21 and 2 4.
  • a communication switching member 26 is interposed between the end surface members 2 2 and 25.
  • the communication switching member 2 6 has a communication hole 2 6 1.
  • the communication switching member 26 can move between the end surface members 2 2 and 25 along the end surface (from the left to the right in the drawing).
  • the closing members 21 and 24 are first removed by the communication switching member 26. Then, the communication hole 2 6 1 of the communication switching member 26 matches the end surface member communication hole of the end surface member 2 2 and 24, so that the first container main body portion 20 and the second container main body portion 2 3 To the communication state (Fig. 4 (b)).
  • the position of the communication hole 26.sub.1 is displaced from the position of the end surface member communication hole, and the space between the first container body 20 and the second container body 23. It will be cut off. Here, it is opposite to the moving direction of the communication switching member 26.
  • a seal member 29 is connected to the opposite end.
  • the seal member 29 is housed in the housing portion 28, and when the communication switching member 26 is moved, the seal member 29 is stretched so as to cover the end surfaces of the end surface members 2 2 and 25, connected to the communication switching member 26. Eventually, the end faces of the end face members 2 2 and 2 4 are covered, and the end face member communication holes are closed.
  • the first container having the first container body 30 and the connecting portion 31 as the first communication passage forming member, the second container body 3 2 and the closing member 3 3 And a second container having a panel 3 4 and a base 3 5.
  • the connecting portion 31 is a tubular member provided at the bottom of the first container main body 30 and is not shown in the drawing, but has a switching cock inside, and allows the liquid in the first container main body 30 to flow. I have control.
  • the second container body 3 2 has a connection hole 3 2 1 on the upper surface. One end of the closing member 3 3 for closing the connection hole 3 2 1 is fixed to the other end of the fixing spring 3 4 on the base 3 5, and is always urged toward the connection hole 3 2 1 side. Yes.
  • the connecting hole 3 2 1 of the second container is closed and kept in a sealed state.
  • the connecting member 31 pushes the closing member 33 into the second container main body 32 and opens the connecting hole 3 21.
  • the first container main body 30 and the second container main body 32 are in communication with each other.
  • the liquid can move into the second container main body 32.
  • the first container main body and the second container main body can be formed by partitioning the first container main body and the second container main body using an elastic body and then deforming the elastic body from the outside. It is also possible to establish communication between the parts. In this case, a gap such as a notch is formed in the elastic body. When the elastic body is not deformed, this gap is brought into close contact with the first container main body and the second container main body, and when the elastic body is deformed, the gap becomes large and It is a communication state between them.
  • At least one of the first container main body and the second container main body, and the wall contacting the other of the first container main body and the second container main body is formed of an elastic body.
  • a tubular needle-like member such as an injection needle can be provided at the other contacting portion.
  • the container on the side where the wall is formed of an elastic body must be sealed before approaching It is kept. Thereafter, the container provided with the needle-like member is brought close to the needle-like member, and the needle-like member is pierced into the elastic body, whereby the two containers can be brought into communication with each other. Thereafter, the needle-like member is pulled out from the elastic body by pulling them apart.
  • the elastic body closes the hole pierced by the needle-like member by its own elasticity, and it becomes a re-sealing state.
  • the separation / extraction member is selected according to the corresponding separation / extraction step.
  • the separation / extraction step is a dissolution step
  • the separation / extraction member is a solution.
  • the separation and extraction process is a liquid-liquid extraction process and a Z or solid-liquid extraction process
  • the separation and extraction member is an extraction liquid.
  • the said separation extraction member in case a separation extraction process is a filtration process is a filtration member.
  • the separation and extraction member when the separation and extraction process is a liquid separation process, includes: (i) a tubular member located at the vicinity of the interface between the two liquids whose tip is separated, and the upper part of the two liquids from the tubular member. Suction means for pulling.
  • a tubular member having a cock at the tip and positioned inside the liquid surface when the lower layer of the two liquids to be separated moves from one container to the other can be employed.
  • Selective filtration is performed using the difference in the degree of lipophilicity and Z or lipophilicity of the two liquids to be separated, and the hydrophilicity of the surface and Z or lipophilicity are controlled.
  • a filtration member can be used.
  • the member (i) absorbs and takes the liquid from the lower container toward the upper container. Specifically, because the tip is near the interface between the two liquids to be separated, the liquid that can be sucked is limited to the upper layer of the two liquids.
  • the member (ii) moves the liquid from the container on the upper side to the container on the lower side as opposed to (i). Specifically, the tip of the lower container of the flow path that connects the upper container and the lower container moves the lower layer of the two liquids from one (upper) container to the other (lower) container. In this case, after all the lower layers of the two liquids have moved down, no more liquid can move to the lower container. It is desirable to provide a cock or the like in the flow path connecting the two containers for both members (i) and (ii).
  • the member (i), which is a member that sucks out the upper layer portion from the lower container to the upper container, is suitable when it is desired to reliably separate the upper layer portion. On the contrary, the lower layer liquid is poured downward.
  • the member (ii) to be discharged is suitable when it is desired to reliably separate the lower layer portion.
  • the member (iii) is a member applicable when the two liquids to be separated have different hydrophilicity and / or lipophilicity. For example, when a hydrophilic (lipophilic) liquid is separated from a mixture of a hydrophilic liquid and a lipophilic liquid, the hydrophilic (lipophilic) surface is filtered through a filter having a hydrophilic (lipophilic) surface. Only lipophilic liquids can be filtered off.
  • the separation and extraction member is an adsorption member.
  • a porous material made of urethane or polyolefin can be used as the adsorbent.
  • the porous resin can adsorb lipophilic liquid.

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  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

A test sample preparation device in which preprocessing can be carried out conveniently under an enclosed state. In the test sample preparation device performing processing on the test sample sequentially while transferring a test sample between unit containers using as many unit containers as required in one or more separation refinement process for separating/extracting an inspection substance by one or more separation extraction process selected from dissolution, liquid-liquid extraction, solid-liquid extraction, filtration, liquid separation, adsorption and reaction, wherein switching is made between communication state and interruption state in order to transfer the test sample between a first container body section (20) and a second container body section (23). Blocking members (21, 24) are removed by moving a communication switching member (26) from an enclosed state (a) to the position (b) and the both are allowed to communicate through a communication hole (261). Subsequently, the communication switching member (26) is moved to the position (c) in order to return them again to an enclosed state, and the communication holes provided in end face members (22, 25) can be blocked by a seal member (29). Since preprocessing can be completed under an enclosed state, measurement can be carried out conveniently in safety.

Description

明細書 試験試料調製装置 技術分野  Technical field
本発明は、 試験試料から被検物質を分離抽出する試験試料調製装置に関する。 背景技術 '  The present invention relates to a test sample preparation apparatus for separating and extracting a test substance from a test sample. Background Technology ''
通常、 ある特定物質の存在の有無や、 その含有量を判別するための手法として は、 クロマトグラフィーや質量分析などを測定原理とする機器分析と呼ばれる手 法が主流である。  Usually, a method called instrumental analysis based on the measurement principle such as chromatography or mass spectrometry is the mainstream for determining the presence or absence of a specific substance and its content.
これらの機器分析では、複数の物質の原子 ·分子レベルでの識別も可能であり、 分析機器を用いない他の分析法と比べて非常に高感度であることが知られている。 し力 し、 高感度であるということは、 分析試料中に含まれる測定対象物質以外 の物質、 すなわち夾雑物も高感度で検出し'てしまう可能性もある。 夾雑物が検出 されると、 場合によっては分析が行えないなどの悪影響が見られ、 分析結果の信 賴性が著しく低下する。 そのため、 測定試料中の夾雑物除去は正確な分析のため に非常に重要である。  In these instrumental analyzes, it is known that a plurality of substances can be identified at the atomic and molecular level, and is extremely sensitive compared to other analytical methods that do not use analytical instruments. However, high sensitivity means that substances other than the measurement target substance contained in the analysis sample, that is, contaminants, may be detected with high sensitivity. When contaminants are detected, adverse effects such as inability to perform analysis are observed in some cases, and the credibility of the analysis results is significantly reduced. Therefore, the removal of contaminants in the measurement sample is very important for accurate analysis.
河川水 ·土壌 ·食品などのさまざまな物質を含む分析試料中に含まれる測定対 象物質を分析する必要がある場合、 機器分析では分析前に、 分析試料中から測定 対象物質を優先的に抽出 ·精製する前処理と呼ばれる工程を行うことが主流であ る。 これら前処理には分析試料の溶解、 液一液抽出、 固一液抽出、 遠心分離、 ゲ ル電気泳動、 蒸留、 カラムクロマトグラフィー、 溶媒の気化による濃縮などの多 種多様な操作を複数組み合わせることが多い。  When it is necessary to analyze the measurement target substance contained in the analysis sample containing various substances such as river water, soil, food, etc., in the instrumental analysis, the measurement target substance is preferentially extracted from the analysis sample before the analysis. · The mainstream is to perform a process called pretreatment for purification. For these pretreatments, a combination of various operations such as dissolution of analysis sample, liquid-liquid extraction, solid-liquid extraction, centrifugation, gel electrophoresis, distillation, column chromatography, and concentration by evaporation of solvent is combined. There are many.
また、 昨今では抗原抗体反応などの生体分子または生物体を使用したパイオア ッセィと呼ばれる手法も普及し始めている。 これらの手法は一般的には抗体の物 質識別能の高さ.を生かし、 測定物質を特異的に検出できる手法として知られてい る。 そのため、 夾雑物の影響は少ないとされている。 しかしながら、 土壌中の重 金属、 キレート化物質など分析試料中に含まれる物質の種類によっては分析結果 の信頼性が著しく低下することがある。 そのため、 バイオアツセィであっても機 器分析に類似した前処理を行う必要が生じる場合もある。 In recent years, a technique called a bioassay using a biomolecule or an organism such as an antigen-antibody reaction has begun to spread. These methods are generally known as methods that can specifically detect a measurement substance by making use of the high substance discrimination ability of antibodies. For this reason, it is said that there is little influence of impurities. However, depending on the type of substances contained in the sample, such as heavy metals and chelating substances in the soil, the analysis results Reliability may be significantly reduced. For this reason, it may be necessary to perform pretreatment similar to instrumental analysis even for bioassays.
このように、 分析試料から測定物質を抽出 ·精製する前処理は、 多様な分析法 におレ、て必要性が高い重要な作業である。  In this way, the pretreatment for extracting and purifying the measurement substance from the analytical sample is an important task that is highly necessary for various analytical methods.
例えば、 P C B汚染物質の測定を例に挙げて説明すると、 文献 1 (低濃度 PCB 汚染物に関する測定法調査中間報告書、 平成 1 7年 5月、 低濃度 P C B汚染物質 対策検討委員会測定法ワーキンググループ: P. 16〜)にあるように、一般的には、 濃縮、 カラムクロマトグラフィ、 酸性処理、 へキサン抽出という作業を繰り返す という高度な研究レベルの手法により精製を行う。 結果として、 これらの公定法 では 8 0 %以上の抽出率と高い再現性が得られることが最大のポイントである。 発明の開示  For example, the measurement of PCB pollutants will be described as an example. Reference 1 (Interim Report on Measurement Methods for Low Concentration PCB Contaminants, May 1995, Low Concentration PCB Contaminant Countermeasures Investigation Committee Working Method In general, purification is performed by advanced research-level methods that repeat the steps of concentration, column chromatography, acid treatment, and hexane extraction, as described in Group: P. 16-). As a result, the most important point of these official methods is that an extraction rate of 80% or more and high reproducibility can be obtained. Disclosure of the invention
(発明が解決しようとする課題)  (Problems to be solved by the invention)
技術背景で述べたが、 分析試料から測定物質を抽出 ·精製する前処理は、 多様 な分析法において必要性が高い重要な作業である。 これら前処理には分析試料の 溶解、.液一液抽出、 固一液抽出、 遠心分離、 ゲル電気泳動、 蒸留、 カラムクロマ トグラフィー、 溶媒の気化による濃縮などの多種多様な操作を複数組み合わせる ことが多い。 これは一例に過ぎないが、 汎用されている分液ロートを用いた液一 液抽出を例に挙げると、 二種の液体を混合した後、 分離した二液間の界面を目視 で確認し、一方の溶液のみを三角フラスコに手作業で回収するという換作を行う。 分液ロートはすりあわせで蓋をしているだけのガラス器具であり、 操作中の液 漏れなどにより操作者が化学薬品に暴露する可能性が高い。 また、 三角フラスコ などの上部開放型のガラス容器を使用する機会も多く、 化学薬品の種類によって は揮発による暴露の可能性も高い。 また、 ガラス器具を洗浄して再使用すること が主流であることから、 洗浄の際に化学薬品に曝露する可能性もある。 ガラス器 具であることから、 破損による曝露の危険性も高い。  As described in the technical background, the pretreatment of extracting and purifying the measurement substance from the analytical sample is an important task that is highly necessary in various analytical methods. These pretreatments can be a combination of a number of different operations such as sample dissolution, liquid-liquid extraction, solid-liquid extraction, centrifugation, gel electrophoresis, distillation, column chromatography, and solvent evaporation. Many. This is only an example, but taking liquid-liquid extraction using a widely used separatory funnel as an example, after mixing two liquids, visually check the interface between the two separated liquids, Only one solution is manually collected in an Erlenmeyer flask. Separation funnels are glass devices that are simply covered with a lid, and the operator is likely to be exposed to chemicals due to liquid leakage during operation. In addition, there are many opportunities to use glass containers with open tops such as Erlenmeyer flasks, and depending on the type of chemical, there is a high possibility of exposure due to volatilization. In addition, since glassware is mainly cleaned and reused, there is a possibility of exposure to chemicals during cleaning. Because it is a glass device, there is a high risk of exposure due to breakage.
また、 前処理は分析試料および測定対象物質ごとに方法が異なるため、 方法が 多岐にわたる。 そのため、 ルーチンワーク化しにくいため自動分析装置等を用い ることも困難であるケースも多く、 操作者の人為ミス等が発生しやすいことも問 題となっている。 In addition, the pretreatment method varies depending on the sample to be analyzed and the substance to be measured. For this reason, there are many cases where it is difficult to use an automatic analyzer because it is difficult to make a routine work, and it is easy to cause human error. It has become a problem.
さらに、 分液ロートでの作業例のように、 作業者の視力、 判断基準、 操作の俊 敏さなどに依存する操作が多く、 作業者ごとに分析結果がバラつくという人為的 な分析精度低下の原因となっている。  In addition, there are many operations that depend on the operator's visual acuity, judgment criteria, operational agility, etc., as in the example of working with a separatory funnel, and the analysis results vary from worker to worker. Cause.
例えば、文献 2 (「絶縁油中のポリ塩素化ビフエニル(PCB)の分析方法規程」、 JEAC 1201- 1991、 (社) 日本電気協会) にあるように、 前処理工程とし" は、 シ リカゲルカラムによる精製や分液ロートを使った液抽出が多く用いられており、 これらの工程は、 手先の器用さ、 俊敏さ、 視力、 判断力など作業者に高度な専門 技術を要する。 従って、 作業者により測定結果がばらつくという問題点があり、 分析の普及を妨げている。  For example, as described in Reference 2 (“Analytical Rules for Polychlorinated Biphenyl (PCB) in Insulating Oil”, JEAC 1201-1991, NEC Corporation), the pretreatment step is “silica gel column. Purification and liquid extraction using a separatory funnel are often used, and these processes require a high level of expertise in the workers such as dexterity, agility, visual acuity, and judgment. As a result, the measurement results vary, which hinders the spread of analysis.
本発明では上記実情に鑑み完成されたものであり、 複雑な前処理が必要な分析 方法において、 密閉状態で且つ簡便に前処理を行うことができる試験試料調製装 置を提供することを解決すべき課題とする。  The present invention has been completed in view of the above circumstances, and solves the problem of providing a test sample preparation apparatus that can easily perform pretreatment in a sealed state in an analysis method that requires complicated pretreatment. It should be a challenge.
(課題を解決するための手段及び発明の効果)  (Means for solving the problems and effects of the invention)
上記課題を解決する本発明の試験試料調製装置は、 固体状乃至液状の試験試料 に対して、 溶解、 液一液抽出、 固一液抽出、 ろ過、 分液、 吸着及び反応のうちか ら選択される 1以上の分離抽出工程により被検物質を分離抽出する試験試料調製 装置である。 これらの分離抽出工程を行うに当たり、 1以上の分離精製工程に必 要な数の単位容器を用い、 該単位容器間で該試験試料を遣り取りしながら順次行 うものである。 つまり、 試験試料は単位容器間を順次移動することで前処理を進 行する。 単位容器内には行う分離抽出工程に対応した分離抽出部材を内部空間に 有することが可能であり、 効率的な分離抽出工程が実現できる。  The test sample preparation apparatus of the present invention that solves the above problems is selected from dissolution, liquid-liquid extraction, solid-liquid extraction, filtration, liquid separation, adsorption, and reaction for a solid or liquid test sample. It is a test sample preparation device that separates and extracts a test substance through one or more separation and extraction processes. In carrying out these separation and extraction steps, the number of unit containers required for one or more separation and purification steps is used, and the test samples are sequentially transferred between the unit vessels. In other words, the test sample is pretreated by moving sequentially between unit containers. The unit container can have a separation and extraction member corresponding to the separation and extraction step to be performed in the internal space, and an efficient separation and extraction step can be realized.
ここで、 前記単位容器は、 容器本体部と連通路形成部材とを備え、  Here, the unit container includes a container body part and a communication path forming member,
該容器本体部は前記試験試料を収容可能に区画された内部空間をもち、 該連通路形成部材は、 該容器本体部に連結し且つ他の単位容器が備える該連通 路形成部材に密閉状態で接続できる接続部と、 密閉状態で接続した状態で自身の 前記容器本体部の内部空間と接続した相手の該容器本体部の内部空間との間で連 通状態及び遮断状態の切り替え可能で且つ該連通状態で該試験試料を遣り取りで きる切替部とをもつ、 ことを特徴とする。 The container main body has an internal space partitioned to accommodate the test sample, and the communication path forming member is connected to the container main body and sealed to the communication path forming member provided in another unit container. It is possible to switch between a connection state and a shut-off state between a connectable connection portion and an internal space of the container main body portion connected to the internal space of the container main body portion connected in a sealed state. A switching unit that can exchange the test sample in a communicating state; It is characterized by that.
つまり、 試験試料に対する前処理をすベて密閉状態で行うために、 試験試料を 移動させていく単位容器間において、 2つの単位容器を密閉状態で接続した後、 内部を連通させるようにすることで、 前処理時に添加する種々の部材 (例えば、 溶解 ·抽出を行う溶媒など) を外部から遮断したまま、 一方の容器から他方の容 器に移動させることが可能になる。 また、 密閉状態を保ったまま両者の間の連通 を遮断して両者を分離できるようにしたことで、 次の前処理工程にも密閉状態の まま、 移行することができる。 密閉状態にて前処理を完了できるので、 P C B汚 染物質の測定など、 試験試料が有害物質にて汚染されているような場合でも安全 に測定を行うことができる。  In other words, in order to perform all pretreatments on the test sample in a sealed state, between the unit containers to which the test sample is moved, the two unit containers are connected in a sealed state, and then the inside is communicated. Thus, it is possible to move various members (for example, a solvent for dissolution / extraction) added at the time of pretreatment from one container to the other container while blocking from the outside. In addition, it is possible to move to the next pretreatment process while keeping the airtight state by blocking the communication between the two while keeping the airtight state so that they can be separated. Since the pretreatment can be completed in a sealed state, measurement can be performed safely even when the test sample is contaminated with harmful substances, such as measurement of PCB contamination.
ここで、 組み合わされる単位容器は同じ物を採用することもできると共に、 前 記複数の単位容器のうちの少なくとも一部は、 残余の該単位容器と異なった構造 を有することもできる。 同じ物を採用するか異なるものを採用するかは、 そこで 行われる分離抽出工程に応じて適正に選択できる。 '  Here, the unit containers to be combined may be the same, and at least a part of the plurality of unit containers may have a different structure from the remaining unit containers. Whether to adopt the same or different ones can be selected appropriately according to the separation and extraction process. '
例えば、 単位容器としては、 順次、 試験'試料や分離抽出部材を移動させる際に 実際に接続を行う単位容器の連通路形成部材間で接続が実現できればその他の部 分 (例えば容器本体部の形状 ·大きさ ·内部に配置された分離抽出部材の種類、 連通路形成部材の構造 (互いに接続できるが同じ構造ではない物) '大きさ) の 構成は特に限定しない。 その他、 前記容器本体部又は前記連通路形成部材に連結 し且つ外部と連通する空気弁を有することもできる。 ここで、 前記容器本体部は 内壁に凹凸部をもつことで、 撹拌効果の向上が期待できるので望ましい。  For example, as for the unit container, other parts (for example, the shape of the container body part) can be used if connection can be realized between the communication path forming members of the unit container that is actually connected when the test sample and separation / extraction member are moved sequentially. · Size · Type of separation / extraction member arranged inside, structure of communication path forming member (thing that can be connected to each other but not the same structure) 'size' is not particularly limited. In addition, an air valve connected to the container body or the communication path forming member and communicating with the outside may be provided. Here, the container body portion is desirable because it has an uneven portion on the inner wall, so that an improvement in the stirring effect can be expected.
ここで、 前記分離抽出工程が溶解工程である場合の前記分離抽出部材としては 溶解液が例示される。 また、 前記分離抽出工程が液一液抽出工程及びノ又は固一 液抽出工程である場合の前記分離抽出部材は抽出液が例示される。 そして、 前記 分離抽出工程がろ過工程である場合の前記分離抽出部材はろ過部材が例示できる。 そして、 前記分離抽出工程が分液工程である場合の前記分離抽出部材は、 先端 が分液する 2液の界面近傍に位置する管状部材と、 該管状部材から前記試験試料 の上層部分を吸引する吸引手段とを備えることが例示される。 また、 前記分離抽 出工程が分液工程である場合の前記分離抽出部材は、 分液する 2液の下層が一方 の容器から他方の容器に移動した場合の液面に先端が位置し内部にコックを持つ 管状部材であるものが例示される。 Here, as the separation and extraction member when the separation and extraction step is a dissolution step, a solution is exemplified. The separation and extraction member in the case where the separation and extraction step is a liquid-liquid extraction step and a solid or single-liquid extraction step is exemplified by an extraction liquid. And when the said separation and extraction process is a filtration process, the said separation and extraction member can illustrate a filtration member. When the separation and extraction step is a liquid separation step, the separation and extraction member includes a tubular member located in the vicinity of the interface between the two liquids separated by the tip, and the upper layer portion of the test sample is sucked from the tubular member And a suction means. In addition, when the separation and extraction process is a liquid separation process, the separation and extraction member has one lower layer of two liquids to be separated. An example is a tubular member having a tip located on the liquid level when moved from one container to the other and having a cock inside.
また、 前記分離抽出工程が分液工程である場合の前記分離抽出部材は、 分液す る 2液の親水性及び Z又は親油性の程度の差を利用して選択的なろ過を行う、 表 面の親水性及び Z又は親油性が制御されたろ過部材が例示される。 更に、 前記分 離抽出工程が吸着工程である場合の前記分離抽出部材は吸着部材が例示される。 互いに接続可能な連通路形成部材の組の具体例を挙げると、  In addition, when the separation and extraction step is a liquid separation step, the separation and extraction member performs selective filtration using a difference in the degree of hydrophilicity and Z or lipophilicity of two liquids to be separated. Examples are filtration members with controlled surface hydrophilicity and Z or lipophilicity. Further, the separation and extraction member in the case where the separation and extraction step is an adsorption step is exemplified by an adsorption member. Specific examples of a set of communication path forming members that can be connected to each other are as follows:
( 1 ) 端面に偏心して設け'られた円筒部材連通孔をもつ円筒部材と、 該円筒部 材の該端面と略同形状であって同程度の偏心をもつて設けられた回動部材連通孔 をもち、 該端面に密着した状態で且つ前記円筒部材連通孔及び前記回動部材連通 孔が一致する位置とずれる位置との間で回動可能に配設されている回動部材とを 備え、 '  (1) A cylindrical member having a cylindrical member communication hole provided eccentrically on the end surface, and a rotating member communication hole having substantially the same shape as the end surface of the cylindrical member and having the same degree of eccentricity. A rotating member disposed in close contact with the end surface and rotatably disposed between a position where the cylindrical member communicating hole and the rotating member communicating hole coincide with a position shifted from each other. '
互いの円筒部材連通孔の位置を合わせ且つ回動部材を接触させて接続し、 それ ぞれの回動部材を合わせて回動させることで連通状態と遮蔽状態との切り替えを 行う部材。 ''  A member that switches between a communication state and a shielding state by aligning the positions of the respective cylindrical member communication holes and contacting and connecting the rotation members, and rotating the respective rotation members together. ''
(.2 ) 互いに接続される 1組の前記連通路形成部材のうち、  (.2) Among the set of communication path forming members connected to each other,
一方の該連通路形成部材は、 端面に設けられた円筒部材連通孔をもつ円筒部材 と、 該円筒部材連通孔を閉塞できる閉塞部材と、 該閉塞部材を該円筒部材の内部 から該円筒部材連通孔に向けて付勢する付勢手段とを備え、  One of the communication path forming members includes a cylindrical member having a cylindrical member communication hole provided on an end surface, a closing member capable of closing the cylindrical member communication hole, and connecting the blocking member from the inside of the cylindrical member to the cylindrical member communication Biasing means for biasing toward the hole,
他方の該連通路形成部材は、 一方の該連通路形成部材に接続するときに、 一方 の該連通路形成部材の前記閉塞部材を前記円筒部材内部に移動させる閉塞部材移 動手段を備える部材。  The other communication path forming member is a member provided with closing member moving means for moving the closing member of one communication path forming member into the cylindrical member when connected to the one communication path forming member.
( 3 ) 互いに接続された 1組の前記連通路形成部材は、 互いに対向する端面に 設けられた端面部材連通孔をもつ 2つの端面部材と、 該端面部材の間であって該 端面部材の該端面に沿って移動可能に介設され、 且つ、 該 2つの端面部材の該端 面部材連通孔の間を連通させる連通孔が形成された連通切り替え部材と、 該連通 切り替え部材の移動に追随し、 該 2つの端面部材の間から該連通切り替え部材を 引き抜いたときに該端面部材連通孔に密着して閉塞する薄膜状のシール部材と、 を備える部材。 ( 4 ) 互いに接続される 1組の前記連通路形成部材のうち、 (3) One set of the communication path forming members connected to each other includes two end surface members having end surface member communication holes provided on opposite end surfaces, and the end surface members between the end surface members. A communication switching member provided movably along the end surface and having a communication hole communicating between the end surface member communication holes of the two end surface members; and following the movement of the communication switching member A thin-film sealing member that closes and closes the end surface member communication hole when the communication switching member is pulled out from between the two end surface members. (4) Of the set of communication path forming members connected to each other,
一方の該連通路形成部材は、弾性材料により端面に形成された密着部材を備え、 他方の該連通路形成部材は、 一方の該連通路形成部材の該密着部材を突き刺し て、 連通状態にする管である針状部材を備える部材が挙げられる。 図面の簡単な説明 ' 第 1図は、本発明に係る試験試料調製装置の第 1実施形態の概略説明図である。 第 2図は、 図 1の装置の作 ίΐを説明する概略図である。  One of the communication path forming members includes a close contact member formed on an end surface of an elastic material, and the other communication path forming member pierces the close contact member of one of the communication path forming members to be in a communication state. The member provided with the acicular member which is a pipe | tube is mentioned. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic explanatory diagram of a first embodiment of a test sample preparation apparatus according to the present invention. FIG. 2 is a schematic diagram for explaining the operation of the apparatus of FIG.
第 3図は、本発明に係る試験試料調製装置の第 2実施形態の概略説明図である。 第 4図は、本発明に係る試験試料調製装置の第 3実.施形態の概略説明図である。 第 5図は、本発明に係る試験試料調製装置の第 4実施形態の概略説明図である。 発明を実施のするための最良の形態  FIG. 3 is a schematic explanatory diagram of a second embodiment of the test sample preparation apparatus according to the present invention. FIG. 4 is a schematic explanatory diagram of a third embodiment of the test sample preparation apparatus according to the present invention. FIG. 5 is a schematic explanatory diagram of a fourth embodiment of the test sample preparation apparatus according to the present invention. BEST MODE FOR CARRYING OUT THE INVENTION
本発明の試験試料調製装置について、 以下、 詳細に^明を行う。 本実施形態の 試験試料調製装置は試験試料中に含まれ 被検物質について複数の工程にて分離 抽出する場合に用いられる装置である。 例えば、 P C B汚染物質の測定における 試験試料の前処理に好適に用いることができる。  The test sample preparation apparatus of the present invention will be described in detail below. The test sample preparation apparatus of this embodiment is an apparatus used when a test substance contained in a test sample is separated and extracted in a plurality of steps. For example, it can be suitably used for pretreatment of test samples in the measurement of PCB contamination.
試験試料としては、 固体状、 液状を問わず対象にできる。 また、 液体中に固体 が分散した懸濁液ゃスラリ一についても対象にすることができる。 試験試料に対 する前処理としては、 '溶解、 液一液抽出、 固一液抽出、 ろ過、 分液、 吸着及ぴ反 応のうちから選択される 1以上の工程に適用することができる。 前処理は最終的 に試験試料中から測定対象である被検物質を分離抽出する工程であり、その際に、 測定に影響を与える不純物を混入しないようにするものである。  Test samples can be solid or liquid. In addition, a suspension in which a solid is dispersed in a liquid can be targeted. The pretreatment for the test sample can be applied to one or more processes selected from dissolution, liquid-liquid extraction, solid-liquid extraction, filtration, liquid separation, adsorption and reaction. The pretreatment is the process of finally separating and extracting the test substance to be measured from the test sample, and at that time, impurities that affect the measurement are not mixed.
分離抽出工程のうち、 溶解は固体状、 懸濁液、 スラリーなどを溶解液に溶解さ せて均質な溶液にする工程である。 液一液抽出は液状若しくは溶解液に溶解させ た試験試料から液体により被検物質を抽出する工程である。 液状の試験試料とは 混合しない液体である抽出液を混合し、 被検物質を抽出液中に移行させた後に、 抽出液を分離することで、 目的とする被検物質を分離できる。 反対に不純物のみ を溶解する抽出液を用いて試験試料がら不純物を除去する工程として採用するこ ともできる。 固一液抽出は固体である試験試料から被検物質を分離抽出する他、 不純物を分離除去する工程として採用することも可能である。 In the separation and extraction process, dissolution is a process in which a solid, suspension, slurry, or the like is dissolved in a solution to make a homogeneous solution. Liquid-liquid extraction is a process in which a test substance is extracted with a liquid from a test sample dissolved in a liquid or solution. The target test substance can be separated by mixing the extract that is not mixed with the liquid test sample, transferring the test substance into the extract, and then separating the extract. Conversely, an extraction solution that dissolves only the impurities is used as a process for removing impurities from the test sample. You can also. Solid-liquid extraction can be used as a process for separating and removing impurities as well as separating and extracting test substances from solid test samples.
ろ過は液体状乃至は溶液状の試験試料から不純物である固体を分離除去したり、 被検物質を含む固体を分離抽出する工程である。 分液は液一液抽出などの工程で 採用した 2つの混合しない溶媒を分離する工程である。 吸着は液状の試験試料か ら不純物を吸着して除去したり、被検物質を吸着により分離抽出する工程である。 被検物質を吸着により分離抽出する場合には吸着させた後に、 何らかの抽出溶媒 (溶出溶媒) により被検物質を溶出させる。 反応は試験試料に対して前処理を行 うにあたって、 試験試料中に液体や固体などの反応試薬を新たに添加する場合で める。 .  Filtration is a process of separating and removing solids that are impurities from a liquid or solution test sample and separating and extracting solids containing a test substance. Separation is a process that separates two unmixed solvents used in processes such as liquid-liquid extraction. Adsorption is a process of adsorbing and removing impurities from a liquid test sample or separating and extracting a test substance by adsorption. When the test substance is separated and extracted by adsorption, the test substance is eluted with some extraction solvent (elution solvent) after adsorption. The reaction should be performed only when a reaction reagent such as a liquid or solid is added to the test sample before pretreatment of the test sample. .
分離抽出工程は、 これらの工程を 1つ又は 2以上組み合わせて用いることで、 試験試料から被検物質を分離抽出し、 分析に影響を与えない程度まで不純物の含 有量を低減させる工程である。 この組み合わせとしては被検物質により大きく異 なるので特に限定できない。 '  The separation and extraction process is a process that separates and extracts the test substance from the test sample by using one or a combination of two or more of these processes, and reduces the impurity content to the extent that it does not affect the analysis. . This combination is not particularly limited because it varies greatly depending on the test substance. '
本実施形態の試験試料調製装置では、 れらの分離抽出工程を行うに当たり、 単位容器を複数個組み合わせて行う。 用いられる複数個の単位容器は全て同じも のであっても良いし、 異な ¾ものであっても良い。 それぞれの単位容器内で行わ れる分離抽出工程は、 それぞれ異なることが多いと考えられるので、 複数の単位 容器は全て同じものではない場合も考えられる。  In the test sample preparation apparatus of this embodiment, when performing these separation and extraction steps, a plurality of unit containers are combined. The plurality of unit containers used may be the same or different. Since the separation and extraction processes performed in each unit container are often considered to be different from each other, there may be cases where a plurality of unit containers are not all the same.
単位容器は、 容器本体部と連通路形成部材と必要に応じて有するその他の構成 要素とをもつ。 容器本体部は試験試料などを収容可能に区画された内部空間をも ち、 分離抽出工程を行う場所である。 分離抽出工程は複数の単位容器内で試験試 料を順次移動させることで行うことができるほ力、 他の単位容器と 1つの単位容 器との間で、 分離抽出に用いる部材 (分離抽出部材) を遣り取りさせることで 1 つの単位容器内で完結させることもできる。 つまり、 それぞれの工程が適用され た後、 試験試料がどの単位容器に移動するかは特に限定しない。  The unit container has a container main body, a communication path forming member, and other constituent elements as necessary. The container body has an internal space partitioned to accommodate test samples and the like, and is a place where the separation and extraction process is performed. The separation and extraction process can be performed by sequentially moving the test sample in a plurality of unit containers, and members used for separation and extraction between other unit containers and one unit container (separation extraction member) ) Can be completed in one unit container. In other words, the unit container to which the test sample is moved after each process is applied is not particularly limited.
容器本体部の大きさ ·内容量は対象となる試験試料の量や操作のし易さなどに より適正に決定できる。 容器本体部の内壁には撹拌効果を向上する目的で凹凸部 をもつことができる。 更に、 内部の液体の流出を制御するために、 空気 (抜き) 弁や加圧手段、 減圧手段を接続しても良い。 加圧手段や減圧手段としてはシリン ジのように、 筒状部材と、 その内部を移動するピストンとの組み合わせや、 スポ イトなどで採用される弾性体から形成されるゴム袋などが採用できる。 The size of the container body • The internal volume can be determined appropriately depending on the amount of test sample to be tested and ease of operation. The inner wall of the container body can have an uneven portion for the purpose of improving the stirring effect. Furthermore, to control the outflow of liquid inside, air (vent) A valve, pressurizing means, or decompressing means may be connected. As the pressurizing means and the depressurizing means, a combination of a cylindrical member and a piston moving inside the cylinder, or a rubber bag formed from an elastic body used for a syringe or the like can be used as in the case of a syringe.
容器本体部には外部から試験試料を導入する導入路である試験試料導入路を設 けることができる。 試験試料が'固体や液体である場合には一般的な蓋などが採用 でき、 液体である場合には更に弾性体から構成される膜なども採用できる。 蓋は 嵌め外しにより開口部を形成し、その開口部から試験試料を導入するものである。 弾 1"生体からなる膜は、 シリン などを用い、 注射針などを突き刺して内部に試験 試料を導入する経路になるものである。  A test sample introduction path which is an introduction path for introducing a test sample from the outside can be provided in the container body. When the test sample is a solid or liquid, a general lid or the like can be used. When the test sample is a liquid, a film made of an elastic material can be used. The lid is opened to form an opening, and the test sample is introduced through the opening. A 1 "biological membrane is a pathway through which a test sample is introduced into the inside using a syringe, etc.
連通路形成部材は接続部と切替部とをもつ。 接続部は容器本体部に連結し且つ 他の単位容器が備える連通路形成部材に密閉状態で接続できる部材である。 切替 部は密閉状態で接続した状態で自身の容器本体部の内部空間と接続した相手の容 器本体部の内部空間との間で連通状態及び遮断状態の切り替え可能で且つ連通状 態で試験試料を遣り取りできる部材である。 それぞれの単位容器内の間で連通状 態になることで、必要な分離抽出部材ゃ試^試料の遺り取りを行うことができる。 接続部はそれぞれの単位容器における容器本体部に設けた開口部にて行う。 こ の開口部の間を密閉状態で接続する。 切替部はこの開口部を開閉できる手段であ る。 従って、 接続部と切替部とは互いに関連性が高い部材であり、 その構成も密 接に関係している。  The communication path forming member has a connection portion and a switching portion. The connecting portion is a member that is connected to the container main body and can be connected in a sealed state to a communication path forming member provided in another unit container. The switching part can be switched between a communication state and a shut-off state between the internal space of the container body part of the container and the internal space of the counterpart container body connected in a sealed state, and the test sample in the communication state. It is a member that can exchange. By connecting to each unit container, the necessary separation and extraction members can be left behind. The connecting portion is made at an opening provided in the container main body of each unit container. Make a sealed connection between these openings. The switching unit is a means that can open and close this opening. Therefore, the connecting portion and the switching portion are highly related members, and their configurations are also closely related.
ここで、 切替部は 2つの単位容器を分離した場合でも、 両者それぞれの密閉性 Here, even when the switching unit separates the two unit containers,
(特に試験試料が移る側の容器や有害物質が存在する側の容器における密閉性) を確保できることが望ましい。 It is desirable to be able to ensure (especially the airtightness of the container on the side where the test sample is transferred and the container on the side where the harmful substances are present).
具体的な連通路形成部材の構成について説明を行う。 連通路形成部材は 2つを 組み合わせて接続する物であるので、 以下、 2つ 1組にて説明を行う。 以下、 一 方を第 1単位容器と称し、 他方を第 2単位容器と便宜的に称する。 第 1 (第 2 ) 単位容器は第 1 (第 2 ) 容器本体部と第 1 (第 2 ) 連通路形成部材とをもつ。  A specific configuration of the communication path forming member will be described. Since the two communication path forming members are connected in combination, the following explanation will be made in pairs. Hereinafter, one is referred to as a first unit container and the other is referred to as a second unit container for convenience. The first (second) unit container has a first (second) container body and a first (second) communication path forming member.
( 1 ) 2つの連通路形成部材の間を接続する構造としては、 円筒部材と回動部 材とを備えるものが挙げらる。 この構造は、 図 1に示すように、 第 1連通路形成 部材の円筒部材 1 0と回動部材 1 1との間、 そして、 第 2連通路形成部材の円筒 部材 1 3と回動部材 1 2との間はそれぞれ回動自在に配設されている。 (1) As a structure for connecting two communication path forming members, a structure including a cylindrical member and a rotating member can be cited. As shown in FIG. 1, this structure is formed between the cylindrical member 10 of the first communication path forming member and the rotating member 11 1, and the cylinder of the second communication path forming member. Between the member 13 and the rotating member 12, each is rotatably arranged.
第 1連通路形成部材における円筒部材 1 0は端面に円筒部材連通孔 1 0 1と端 面から突出する回動規制ピン 1 0 2が形成されている。 円筒部材連通孔 1 0 1は 円筒部材 1 0の端面において偏心して形成されている。 円筒部材 1 0の端面には 回動部材 1 1が回動自在に設けられている。 回動部材 1 1は回動部材連通孔 1 1 1と円筒部材 1 0の反対方向に突出する回動規制ピン 1 1 2と回動規制溝 1 1 3 とをもつ。 円筒部材 1 0の回動規制ピン 1 0 2は回動部材 1 1の回動規制溝 1 1 3内に挿入されて、 図 2 ( a ) に示すように、 (a— 1 ) と (a— 2 ) との間で 回動範囲を規制している。 (a— 1 ) の位置は円筒部材 1 0の円筒部材連通孔 1 0 1と回動部材連通孔 1 1 1との間がずれて遮断状.態になっている。 ( a— 2 ) の位置は (a— 1 ) の位置から反時計回りに 9 0 ° 回転した状態で、 円筒部材 1 0の円筒部材連通孔 1 0 1と回動部材連通孔 1 1 1との間が一致して連通状態に なっている。  The cylindrical member 10 in the first communication path forming member has a cylindrical member communication hole 10 1 and a rotation restricting pin 10 2 protruding from the end surface on the end surface. The cylindrical member communication hole 10 1 is formed eccentrically on the end face of the cylindrical member 10. A rotating member 11 is rotatably provided on the end surface of the cylindrical member 10. The rotating member 1 1 has a rotating member communication hole 1 1 1, a rotation restricting pin 1 1 2 protruding in the opposite direction of the cylindrical member 10, and a turn restricting groove 1 1 3. The rotation restricting pin 10 0 2 of the cylindrical member 10 is inserted into the rotation restricting groove 1 1 3 of the rotating member 1 1, and as shown in FIG. 2 (a), (a-1) and (a — The range of rotation is restricted between 2). The position of (a-1) is in a cut-off state because the cylindrical member communication hole 10 0 1 of the cylindrical member 10 and the rotating member communication hole 1 1 1 are displaced. The position of (a-2) is rotated 90 ° counterclockwise from the position of (a-1), and the cylindrical member communication hole 1 0 1 and the rotation member communication hole 1 1 1 Are in communication with each other.
第 2連通路形成部材における円筒部材 1 3は端面に円筒部材連通孔 1 3 1と回 動規制溝 1 3 2が形成されている。 円筒部材 1 3の端面には回動部材 1 2が回動 自在に設けられている。 回動部材 1 2は回動部材連通孔 1 2 1と円筒部材 1 3側 に突出する回動規制ピン 1 2 2と回動規制溝 1 2 3とをもつ。 回動部材 1 2の回 動規制ピン 1 2 2は円筒部材 1 3の回動規制溝 1 3 2内に挿入されて、図 2 ( c ) に示すように、 (c— l ) と (c— 2 ) との間で回動範囲を規制している。 (c 一 1 ) の位置は円筒部材 1 3の円筒部材連通孔 1 3 1と回動部材連通孔 1 2 1と の間がずれて遮断状態になっている。 (c一 2 ) の位置は (c一 1 ) の位置から 反時計回りに 9 0 ° 回転した状態で、 円筒部材 1 3の円筒部材連通孔 1 3 1と回 動部材連通孔 1 2 1との間が一致して連通状態になっている。  The cylindrical member 13 in the second communication path forming member has a cylindrical member communication hole 13 1 and a rotation restricting groove 13 2 formed on the end face. A rotating member 12 is rotatably provided on the end surface of the cylindrical member 13. The rotation member 1 2 has a rotation member communication hole 1 2 1, a rotation restricting pin 1 2 2 protruding to the cylindrical member 1 3 side, and a rotation restricting groove 1 2 3. The rotation restricting pin 1 2 2 of the rotating member 1 2 is inserted into the rotation restricting groove 1 3 2 of the cylindrical member 1 3, and as shown in FIG. 2 (c), (c− l) and (c — The range of rotation is restricted between 2). The position of (c 1 1) is in a blocked state because the cylindrical member communication hole 13 1 of the cylindrical member 13 is displaced from the rotating member communication hole 1 2 1. The position of (c 1 2) is rotated 90 ° counterclockwise from the position of (c 1 1), and the cylindrical member communication hole 1 3 1 and the rotating member communication hole 1 2 1 Are in communication with each other.
第 1連通路形成部材における回動部材 1 1と第 2連通路形成部材における回動 部材 1 2との間で重ね合わせることで、 第 1容器と第 2容器との間の接続が行わ れる。 第 1連通路形成部材の回動部材 1 1における回動規制ピン 1 1 2は第 2連 通路形成部材における回動規制溝 1 2 3内に挿入されて、 図 2 ( b ) に示すよう に、 (b— 1 ) と (b— 2 ) との間で回動範囲を規制している。 (b— 1 ) の位 置は回動部材連通孔 1 1 1と回動部材連通孔 1 2 1との間がずれて遮断状態にな つている。 (b— 2) の位置は (b— 1) の位置から反時計回りに 90° 回転し た状態で、 回動部材連通孔 1 1 1と回動部材連通孔 1 2 1との間が一致して連通 状態になっている。 The first container and the second container are connected by overlapping the rotating member 11 in the first communication path forming member and the rotating member 12 in the second communication path forming member. As shown in FIG. 2 (b), the rotation restricting pin 1 1 2 in the rotating member 11 of the first communication path forming member is inserted into the rotation restricting groove 1 2 3 in the second communication path forming member. , (B-1) and (b-2) restrict the rotation range. The position of (b-1) is in the blocked state because the rotation member communication hole 1 1 1 and the rotation member communication hole 1 2 1 are displaced. It is. The position of (b-2) is rotated 90 ° counterclockwise from the position of (b-1), and the rotation member communication hole 1 1 1 and the rotation member communication hole 1 2 1 are the same. Then it is in communication.
従って、 全体としては、 第 1連通路形成部材における円筒部材連通孔 1 0 1及 び回動部材連通孔 1 1 1、 第 2連通路形成部材における回動部材連通孔 1 2 1及 び円筒部材連通孔 1 3 1の間がすべて一致する ( a— 2 ) 、 (b -2) 及び ( c - 2) の状態 (第 2の状態) から、 時計回りに 3 6 0° 回動させることで、 すべ ての連通孔 1 0 1、 1 1 1、 ί 2 1及び 1 3 1の間がすべてずれている(a— 1)、 Therefore, as a whole, the cylindrical member communication hole 10 1 and the rotation member communication hole 1 1 1 in the first communication path forming member, the rotation member communication hole 1 2 1 in the second communication path formation member and the cylindrical member From the state (second state) of (a-2), (b-2) and (c-2) where all the communication holes 1 3 1 are coincident, it is possible to rotate 3 60 degrees clockwise. , All communication holes 1 0 1, 1 1 1, ί 2 1 and 1 3 1 are all off (a-1),
(b- 1) 、 そして (c一 1) の状態 (第 1の状態) にまで変化させることがで さる。 It is possible to change the state to (b-1) and (c 1 1) (first state).
従って、 遮断状態である第 1の状態で、 第 1容器の第 1連通路形成部材と第 2 容器の第 2連通路形成部材との間を接続した上で、 第 2の状態にまで両者を回動 させることで第 1容器内と第 2容器内とが連通した連通状態にさせて、 分離抽出 工程に必要な分離抽出部材の遣り取りを行った後、 反対側に回動させることで第 1の状態にして再度、 遮断状態にするこ'とが可能になる。  Therefore, in the first state, which is the shut-off state, the first communication path forming member of the first container and the second communication path forming member of the second container are connected, and then both are brought to the second state. By rotating, the first container and the second container are in communication with each other, and after exchanging the separation and extraction members necessary for the separation and extraction process, the first container is rotated to the opposite side. It becomes possible to turn it into a shut-off state again.
更に、 円筒部材の端面や回動部材の表面には、 汚染防止のためにワイパー (図 略) を設けることもできる。 ワイパーはそれぞれの表面であって半径方向に延ぴ る線状の突起として設けることができる。 円筒部材の端面及び回動部材、 又は、 回動部材同士の間にこの突起を設けることで、 それぞれの間を回動させる際に突 起が接する相手側の表面に残存する液体などを拭き取ることができる。  Furthermore, a wiper (not shown) can be provided on the end face of the cylindrical member or the surface of the rotating member to prevent contamination. The wiper can be provided as a linear protrusion extending radially on each surface. By providing this protrusion between the end face of the cylindrical member and the rotating member, or between the rotating members, the liquid remaining on the surface of the other side where the protrusion comes into contact when rotating between them is wiped off. Can do.
•また、 第 2連通路形成部材としては、 上記構成に代えて、 図 3に示す構成を採 用することができる。 まず、 第 1連通路形成部材における円筒部材の端面 1 0 ' に円筒部材連通孔 1 0 1 ' が設けられ、 更に、 回動部材連通孔 1 1 1 ' が設けら れた回動部材 1 1 ' がその端面 1 0, に回動自在に設けられている点では上記構 成と同じである。  • As the second communication path forming member, the configuration shown in FIG. 3 can be adopted instead of the above configuration. First, a cylindrical member communication hole 1 0 1 ′ is provided on the end face 10 ′ of the cylindrical member in the first communication path forming member, and further, a rotating member 1 1 provided with a rotating member communication hole 1 1 1 ′. It is the same as the above configuration in that 'is rotatably provided on its end face 10,.
また、 第 2連通路形成部材における円筒部材の端面 1 3 ' にも円筒部材連通孔 The cylindrical member communication hole is also formed in the end surface 1 3 ′ of the cylindrical member in the second communication path forming member.
1 3 1, が設けられ、 更に、 回動部材連通孔 1 2 1, が設けられた回動部材 1 21 3 1, and a rotating member communication hole 1 2 1, and a rotating member 1 2
' がその端面 1 3 ' に回動自在に設けられている点でも上記構成と同じである。 これら第 1連通路形成部材と第 2連通路形成部材とを突き合わせて接続する。 両者の接続は円筒部材の端面 1 0 ' における円筒部材連通孔 1 0 1 ' の位置と円 筒部材の端面 1 3 'における円筒部材連通孔 1 3 1 'の位置とを合わせると共に、 回動部材 1 1 ' における回動部材連通孔 1 1 1 ' の位置と回動部材 1 2, におけ る回動部材連通孔 1 2 1 ' の位置とについても合わせるように接続する。 It is the same as the above configuration in that 'is rotatably provided on the end face 1 3'. The first communication path forming member and the second communication path forming member are abutted and connected. The connection between the two is made by aligning the position of the cylindrical member communication hole 1 0 1 ′ on the end face 10 ′ of the cylindrical member with the position of the cylindrical member communication hole 1 3 1 ′ on the end face 1 3 ′ of the cylindrical member, Connect so that the position of the rotating member communication hole 1 1 1 'in 1 1 ′ and the position of the rotating member communication hole 1 2 1 ′ in rotating member 1 2, also match.
そうすると、 回動部材 1 1 ' '及び 1 2 ' のそれぞれに設けた回動爪 1 1 4, 及 ぴ 1 2 4, の位置も合うことになる。 この回動爪 1 1 4 ' 及び 1 2 4 ' を使って 回動部材 1 1 ' 及び 1 2 ' を回動させ、 円筒部材連通孔 1 0 1 ' 、 回動部材連通 孔 1 1 1 ' 、 回動部材連通孔 1 2 1 ' 及び円筒部材連通孔 1 3 1 ' の位置を一致 させることで、 第 1容器と第 2容器との間を連通状態にすることができる。 更に、 回動爪 1 1 4 ' 及び 1 2 4 ' を使って回動部材 1 1, 及ぴ 1 2, を回動 させ、 円筒部材連通孔 1 0 1 ' 、 回動部材連通孔 1 1 1 ' 、 回動部材連通孔 1 2 1, 及び円筒部材連通孔 1 3 1 ' の位置をずらすことで、 第 1容器と第 2容器と の間を遮断状態にすることができる。  Then, the positions of the rotating claws 1 1 4 and 1 2 4 provided on the rotating members 1 1 ′ and 1 2 ′ are also aligned. Using the rotating claws 1 1 4 ′ and 1 2 4 ′, the rotating members 1 1 ′ and 1 2 ′ are rotated, and the cylindrical member communication holes 1 0 1 ′, the rotating member communication holes 1 1 1 ′, By aligning the positions of the rotation member communication hole 1 2 1 ′ and the cylindrical member communication hole 1 3 1 ′, the first container and the second container can be in communication. Further, the rotating claws 1 1 4 ′ and 1 2 4 ′ are used to rotate the rotating members 1 1 and 1 2, and the cylindrical member communicating holes 1 0 1 ′ and the rotating member communicating holes 1 1 1 By shifting the positions of the rotation member communication hole 1 2 1 and the cylindrical member communication hole 1 3 1 ′, the first container and the second container can be shut off.
•更に、 第 2連通路形成部材としては、 上記構成に代えて、 図 4に示す構成を採 用することができる。 図 4は、 第 1容器 ϊ第 2容器とを組み合わせた状態を示し ている。 第 1容器本体部 2 0と第 2容器本体部 2 3とは端面部材 2 2と端面部材 2 5とを所定間隔を介して対向するように配設している。  • Furthermore, instead of the above configuration, the configuration shown in FIG. 4 can be adopted as the second communication path forming member. FIG. 4 shows a state where the first container and the second container are combined. The first container main body 20 and the second container main body 23 are arranged so that the end surface member 22 and the end surface member 25 are opposed to each other with a predetermined interval.
端面部材 2 2及ぴ 2 5はそれぞれ端面部材連通孔をもち、 その連通孔は閉塞部 材 2 1及ぴ 2 4にて閉塞されている。 端面部材 2 2及び 2 5の間には連通切り替 ぇ部材 2 6を介装している。 連通切り替え部材 2 6は連通孔 2 6 1をもつ。 連通 切り替え部材 2 6は端面部材 2 2及び 2 5の間で端面に沿って (図面左方から右 方) 移動可能である。  Each of the end surface members 2 2 and 25 has an end surface member communication hole, and the communication holes are closed by the closing members 21 and 2 4. A communication switching member 26 is interposed between the end surface members 2 2 and 25. The communication switching member 2 6 has a communication hole 2 6 1. The communication switching member 26 can move between the end surface members 2 2 and 25 along the end surface (from the left to the right in the drawing).
連通切り替え部材 2 6を移動すると、 まず閉塞部材 2 1及ぴ 2 4が連通切り替 ぇ部材 2 6により取り外される。 そして、 連通切り替え部材 2 6の連通孔 2 6 1 が端面部材 2 2及ぴ 2 4の端面部材連通孔と一致することで、 第 1容器本体部 2 0及び第 2容器本体部 2 3の間を連通状態にする (図 4 ( b ) ) 。  When the communication switching member 26 is moved, the closing members 21 and 24 are first removed by the communication switching member 26. Then, the communication hole 2 6 1 of the communication switching member 26 matches the end surface member communication hole of the end surface member 2 2 and 24, so that the first container main body portion 20 and the second container main body portion 2 3 To the communication state (Fig. 4 (b)).
その後、 更に連通切り替え部材 2 6を移動させると、 連通孔 2 6 1の位置が端 面部材連通孔の位置からずれて、 第 1容器本体部 2 0及び第 2容器本体部 2 3の 間が遮断状態になる。 ここで、 連通切り替え部材 2 6の移動する方向に対して反 対側の端部にはシール部材 2 9が接続されている。 シール部材 2 9は収納部 2 8 に収納されており、 連通切り替え部材 2 6を移動させると、 連通切り替え部材 2 6に連られて端面部材 2 2及ぴ 2 5の端面を覆うように引き延ばされ、 最終的に は端面部材 2 2及ぴ 2 4の端面を覆って、 それぞれの端面部材連通孔を閉塞する ことになる。 Thereafter, when the communication switching member 26 is further moved, the position of the communication hole 26.sub.1 is displaced from the position of the end surface member communication hole, and the space between the first container body 20 and the second container body 23. It will be cut off. Here, it is opposite to the moving direction of the communication switching member 26. A seal member 29 is connected to the opposite end. The seal member 29 is housed in the housing portion 28, and when the communication switching member 26 is moved, the seal member 29 is stretched so as to cover the end surfaces of the end surface members 2 2 and 25, connected to the communication switching member 26. Eventually, the end faces of the end face members 2 2 and 2 4 are covered, and the end face member communication holes are closed.
•そして、 図 5に示すように、 第 1容器本体部 3 0と第 1連通路形成部材として の連結部位 3 1とをもつ第 1容器と、 第 2容器本体部 3 2と閉塞部材 3 3とパネ 3 4と基台 3 5とをもつ第 2容器との組み合わせが挙げられる。 連結部位 3 1は 第 1容器本体部 3 0の底に設けられた管状の部材で図面には示さないが、 内部に 切り替えコックを有し、 第 1容器本体部 3 0内の液体の流通を制御している。 第 2容器本体部 3 2は上面に連結孔 3 2 1を有する。 この連結孔 3 2 1を閉塞 する閉塞部材 3 3は基台 3 5上に一端部が固定バネ 3 4の他端部に固定されてお り、 常に連結孔 3 2 1側に付勢されている。  As shown in FIG. 5, the first container having the first container body 30 and the connecting portion 31 as the first communication passage forming member, the second container body 3 2 and the closing member 3 3 And a second container having a panel 3 4 and a base 3 5. The connecting portion 31 is a tubular member provided at the bottom of the first container main body 30 and is not shown in the drawing, but has a switching cock inside, and allows the liquid in the first container main body 30 to flow. I have control. The second container body 3 2 has a connection hole 3 2 1 on the upper surface. One end of the closing member 3 3 for closing the connection hole 3 2 1 is fixed to the other end of the fixing spring 3 4 on the base 3 5, and is always urged toward the connection hole 3 2 1 side. Yes.
従って、 通常は第 2容器の連結孔 3 2 1は閉塞し^状態になっており、 密閉状 態が保たれる。 そして、 第 2容器の上方'から第 1容器を接近させると、 連結部位 3 1により閉塞部材 3 3が第 2容器本体部 3 2の内部に押し入れられて連結孔 3 2 1が開口する。 その結果、 第 1容器本体部 3 0と第 2容器本体部 3 2との間は 連通状態になり、 連結部位 3 1にも受けられた切り替えコックの操作によって第 1容器本体部 3 0内の液体は第 2容器本体部 3 2内に移動することができる。 •その他にも、 弾性体を用いて第 1容器本体部と第 2容器本体部との間を区画し た上で、 弾性体を外部から変形させることで第 1容器本体部及び第 2容器本体部 の間を連通状態とすることもできる。 この場合に、 弾性体には切り欠きなどの隙 間を形成する。 この隙間は弾性体が変形していない場合には、 密着して第 1容器 本体部及び第 2容器本体部の間を遮断状態とし、 弾性体を変形した場合には隙間 が大きくなつて両者の間を連通状態にするものである。  Therefore, normally, the connecting hole 3 2 1 of the second container is closed and kept in a sealed state. When the first container is approached from above the second container, the connecting member 31 pushes the closing member 33 into the second container main body 32 and opens the connecting hole 3 21. As a result, the first container main body 30 and the second container main body 32 are in communication with each other. The liquid can move into the second container main body 32. • In addition, the first container main body and the second container main body can be formed by partitioning the first container main body and the second container main body using an elastic body and then deforming the elastic body from the outside. It is also possible to establish communication between the parts. In this case, a gap such as a notch is formed in the elastic body. When the elastic body is not deformed, this gap is brought into close contact with the first container main body and the second container main body, and when the elastic body is deformed, the gap becomes large and It is a communication state between them.
また、 第 1容器本体部又は第 2容器本体部のうちの少なくとも一方であって、 第 1容器本体部又は第 2容器本体部のうちの他方に接する壁を部分を弾性体で形 成した上で、 他方の接する部分に注射針のような管状の針状部材を設けることも できる。 両者の間を接近させる前は弾性体で壁を形成した側の容器は密閉状態が 保たれている。 その後、 針状部材を設けた容器を接近させて、 針状部材を弾性体 に突き刺すことで、 両者の容器の間を連通状態にすることができる。 その後、 両 者を引き離すことで、 針状部材は弾性体から引き抜かれる。 弾性体は自身の弾性 により針状部材が突き刺さった孔を塞ぎ、 再ぴ密閉状態になる。 In addition, at least one of the first container main body and the second container main body, and the wall contacting the other of the first container main body and the second container main body is formed of an elastic body. Thus, a tubular needle-like member such as an injection needle can be provided at the other contacting portion. The container on the side where the wall is formed of an elastic body must be sealed before approaching It is kept. Thereafter, the container provided with the needle-like member is brought close to the needle-like member, and the needle-like member is pierced into the elastic body, whereby the two containers can be brought into communication with each other. Thereafter, the needle-like member is pulled out from the elastic body by pulling them apart. The elastic body closes the hole pierced by the needle-like member by its own elasticity, and it becomes a re-sealing state.
分離抽出部材は対応する分離抽出工程に応じて選択される。 例えば、 分離抽出 工程が溶解工程である場合の分離抽出部材は溶解液である。 また、 分離抽出工程 が液一液抽出工程及ぴ Z又は固一液抽出工程である場合の分離抽出部材は抽出液 である。 そして、 分離抽出工程がろ過工程である場合の前記分離抽出部材はろ過 部材である。  The separation / extraction member is selected according to the corresponding separation / extraction step. For example, when the separation / extraction step is a dissolution step, the separation / extraction member is a solution. In addition, when the separation and extraction process is a liquid-liquid extraction process and a Z or solid-liquid extraction process, the separation and extraction member is an extraction liquid. And the said separation extraction member in case a separation extraction process is a filtration process is a filtration member.
また、分離抽出工程が分液工程である場合の分離抽出部材は、 (i)先端が分液す る 2液の界面近傍に位置する管状部材と、 その管状部材から 2液の上層部分を吸 引する吸引手段とを備えることができる。 また、 (ii)分液する 2液の下層が一方 の容器から他方の容器に移動した場合の液面に先端が位置し内部にコックを持つ 管状部材が採用できる。更に、 (iii)分液する 2液の親'水性及ぴ Z又は親油性の程 度の差を利用して選択的なろ過を行う、 表面の親水性及ぴ Z又は親油性が制御さ れた.ろ過部材が採用できる。  In addition, when the separation and extraction process is a liquid separation process, the separation and extraction member includes: (i) a tubular member located at the vicinity of the interface between the two liquids whose tip is separated, and the upper part of the two liquids from the tubular member. Suction means for pulling. In addition, (ii) a tubular member having a cock at the tip and positioned inside the liquid surface when the lower layer of the two liquids to be separated moves from one container to the other can be employed. In addition, (iii) Selective filtration is performed using the difference in the degree of lipophilicity and Z or lipophilicity of the two liquids to be separated, and the hydrophilicity of the surface and Z or lipophilicity are controlled. A filtration member can be used.
(i)の部材は下側にある容器から上側にある容器に向けて液体を吸レ、取るもの である。 具体的には、 先端部が分液すべき 2液の界面近傍にあることで、 吸い込 むことができる液体は 2液の上層部分に限定される。  The member (i) absorbs and takes the liquid from the lower container toward the upper container. Specifically, because the tip is near the interface between the two liquids to be separated, the liquid that can be sucked is limited to the upper layer of the two liquids.
(ii)の部材は(i)とは反対に上側にある容器から下側にある容器に向けて液体 を移動させるものである。 具体的には、 上側の容器と下側の容器とを連通する流 路の下側の容器における先端が、 2液の下層が一方(上側)の容器から他方 (下側) の容器に移動した場合の液面の位置に設定していることで、 2液の下層がすべて 下側に移動した後はそれ以上液体が下側の容器に移動することができなくなる。 (i)及ぴ(ii)の両部材とも 2つの容器を連通する流路にはコックなどを設けるこ とが望ましい。 なお、 下側の容器から上側の容器に上層部分を吸い出す部材であ る(i)の部材は上層部分を確実に分離することを望む場合に好適であり、反対に下 方向に下層の液体を流出させる(ii)の部材は下層部分を確実に分離することを望 む場合に好適である。 ' (iii)の部材は分液すべき 2液の親水性及び/又は親油性が異なる場合に適用 できる部材である。例えば親水性の液体と親油性の液体との混合物から親水性 (親 油性)の液体を分離する場合には表面を親水化 (親油化)したフィルタ一によりろ 過することで、 親水性 (親油性)の液体だけをろ過分離することができる。 The member (ii) moves the liquid from the container on the upper side to the container on the lower side as opposed to (i). Specifically, the tip of the lower container of the flow path that connects the upper container and the lower container moves the lower layer of the two liquids from one (upper) container to the other (lower) container. In this case, after all the lower layers of the two liquids have moved down, no more liquid can move to the lower container. It is desirable to provide a cock or the like in the flow path connecting the two containers for both members (i) and (ii). The member (i), which is a member that sucks out the upper layer portion from the lower container to the upper container, is suitable when it is desired to reliably separate the upper layer portion. On the contrary, the lower layer liquid is poured downward. The member (ii) to be discharged is suitable when it is desired to reliably separate the lower layer portion. ' The member (iii) is a member applicable when the two liquids to be separated have different hydrophilicity and / or lipophilicity. For example, when a hydrophilic (lipophilic) liquid is separated from a mixture of a hydrophilic liquid and a lipophilic liquid, the hydrophilic (lipophilic) surface is filtered through a filter having a hydrophilic (lipophilic) surface. Only lipophilic liquids can be filtered off.
分離抽出工程が吸着工程である場合の分離抽出部材は吸着部材である。例えば、 親水性の液体と親油性の液体とが混合されている試験試料から親油性の液体.を吸 着する工程の場合に、 吸着剤としてウレタンやポリオレフイン製の多孔質材料を 採用することで、 その多孔 ®により親油性の液体を吸着することができる。  When the separation and extraction process is an adsorption process, the separation and extraction member is an adsorption member. For example, in the process of adsorbing a lipophilic liquid from a test sample in which a hydrophilic liquid and a lipophilic liquid are mixed, a porous material made of urethane or polyolefin can be used as the adsorbent. The porous resin can adsorb lipophilic liquid.

Claims

WO 2007/097246 請求の範囲 WO 2007/097246 Claims
1 . 固体状乃至液状の試験試料に対して、 溶解、 液一液抽出、 固一液抽出、 ろ 過、 分液、 吸着及び反応のうちから選択される 1以上の分離抽出工程により被検 物質を分離抽出する 1以上の分離精製工程に必要な数の単位容器を用い、 該単位 容器間で該試験試料を遣り取りしながら順次行う試験試料調製装置であって、 前記単位容器は、 容器本体部と連通路形成部材とを備え、 1. For a solid or liquid test sample, a test substance is obtained by one or more separation / extraction steps selected from dissolution, liquid-liquid extraction, solid-liquid extraction, filtration, liquid separation, adsorption and reaction. 1 is a test sample preparation apparatus that uses a number of unit containers necessary for one or more separation and purification steps and sequentially transfers the test sample between the unit containers, wherein the unit container includes a container body portion. And a communication path forming member,
該容器本体部は前記試験試料を収容可能に区画された内部空間をもち、 該連通路形成部材は、 該容器本体部に連結し且つ他の単位容器が備える該連通 路形成部材に密閉状態で接続できる接続部と、 密閉状態で接続した状態で自身の 前記容器本体部の内部空間と接続した相手の該容器本体部の内部空間との間で連 通状態及び遮断状態の切り替え可能で且つ該連通状態で該試験試料を遣り取りで きる切替部とをもつ、  The container main body has an internal space partitioned to accommodate the test sample, and the communication path forming member is connected to the container main body and sealed to the communication path forming member provided in another unit container. It is possible to switch between a connection state and a shut-off state between a connectable connection portion and an internal space of the container main body portion connected to the internal space of the container main body portion connected in a sealed state. A switching unit that can exchange the test sample in a communicating state;
ことを特徴とする試験試料調製装置。  The test sample preparation apparatus characterized by the above-mentioned.
2 . 前記分離抽出工程に用い且つ前記本体部の内部空間内に配設される分離抽 出部材を有する請求項 1に記載の試験試料調製装置。  2. The test sample preparation apparatus according to claim 1, further comprising a separation extraction member used in the separation extraction step and disposed in an internal space of the main body.
3 . 前記容器本体部若しくは前記連通路形成部材に連結し且つ外部と連通する 空気弁を有するか、.又は、 前記容器本体部は内壁に凹凸部をもつ請求項 1又は 2 に記載の試験試料調製装置。  3. An air valve connected to the container body or the communication path forming member and communicating with the outside, or the test body according to claim 1 or 2, wherein the container body has an uneven portion on an inner wall. Preparation equipment.
4 . 前記分離抽出部材は、  4. The separation and extraction member is
前記分離抽出工程が溶解工程である場合は溶解液であり、  When the separation and extraction step is a dissolution step, it is a dissolution solution,
前記分離抽出工程が液一液抽出工程及び Z又は固一液抽出工程である場合は抽 出液であり、  If the separation and extraction process is a liquid-liquid extraction process and a Z or solid-liquid extraction process, it is an extraction liquid,
前記分離抽出工程がろ過工程である場合はろ過部材である請求項 1〜 3のいず れかに記載の試験試料調製装置。  The test sample preparation apparatus according to any one of claims 1 to 3, wherein when the separation and extraction step is a filtration step, the separation member is a filtration member.
5 . 前記分離抽出工程が分液工程である場合の前記分離抽出部材は、  5. The separation and extraction member when the separation and extraction step is a liquid separation step,
先端が分液する 2液の界面近傍に位置する管状部材と、 該管状部材から前記試 験試料の上層部分を吸引する吸引手段とを備える力 又は、  A force provided with a tubular member located near the interface between the two liquids, the tip of which separates, and suction means for sucking the upper layer portion of the test sample from the tubular member, or
分液する 2液の下層が一方の容器から他方の容器に移動した場合の液面に先端
Figure imgf000018_0001
Separation The tip of the two-liquid lower layer moves from one container to the other.
Figure imgf000018_0001
が位置し内部にコックを持つ管状部材を備える請求項 1〜 4のいずれかに記載の 試験試料調製装置。 The test sample preparation apparatus according to any one of claims 1 to 4, further comprising a tubular member that is positioned and has a cock inside.
6 . 前記分離抽出工程が分液工程である場合の前記分離抽出部材は、 分液する 2液の親水性及び 又は親油性の程度の差を利用して選択的なろ過を行う、 表面 の親水性及び/又は親油性が制御されたろ過部材である請求項 1〜 5のいずれか に記載の試験試料調製装置。 '  6. When the separation and extraction step is a liquid separation step, the separation and extraction member performs selective filtration by utilizing the difference in hydrophilicity and / or lipophilicity of the two liquids to be separated. The test sample preparation apparatus according to any one of claims 1 to 5, wherein the test sample preparation apparatus is a filtration member with controlled properties and / or lipophilicity. '
7 . 前記分離抽出工程が吸着工程である場合の前記分離抽出部材は吸着部材で ある請求項 1〜 6のいずれ に記載の試験試料調製装置。  7. The test sample preparation apparatus according to any one of claims 1 to 6, wherein the separation and extraction member when the separation and extraction step is an adsorption step is an adsorption member.
8 . 前記連通路形成部材は、  8. The communication path forming member is
端面に偏心して設けられた円筒部材連通孔をもつ円筒部材と、 該円筒部材の該 端面と略同形状であって同程度の偏心をもって設けられた回動部材連通孔をもち、 該端面に密着した状態で且つ前記円筒部材連通孔及ぴ前記回動部材連通孔がー致 する位置とずれる位置との間で回動可能に配設されている回動部材とを備え、 互いの円筒部材連通孔の位置を合わせ且つ回動部材を接触させて接続し、 それ ぞれの回動部材を合わせて回動させるこ 'とで連通状態と遮蔽状態との切り替えを 行う.請求項 1〜 7のいずれかに記載の試験試料調製装置。  A cylindrical member having a cylindrical member communication hole provided eccentrically on the end surface, and a rotating member communication hole having substantially the same shape as the end surface of the cylindrical member and provided with the same degree of eccentricity, are in close contact with the end surface And a rotating member arranged to be rotatable between a position where the cylindrical member communicating hole and the rotating member communicating hole are aligned with a position shifted from each other. The communication state and the shielding state are switched by aligning the positions of the holes and connecting the rotating members in contact with each other to rotate the respective rotating members together. The test sample preparation apparatus according to any one of the above.
9 . 互レヽに接続される 1組の前記連通路形成部材のうち、  9. Of the set of communication path forming members connected to each other,
一方の該連通跨形成部材は、 端面に設けられた円筒部材連通孔をもつ円筒部材 と、 該円筒部材連通孔を閉塞できる閉塞部材と、 該閉塞部材を該円筒部材の内部 から該円筒部材連通孔に向けて付勢する付勢手段とを備え、  One of the communication straddling members includes a cylindrical member having a cylindrical member communication hole provided on an end surface, a closing member capable of closing the cylindrical member communication hole, and connecting the blocking member from the inside of the cylindrical member to the cylindrical member communication Biasing means for biasing toward the hole,
他方の該連通路形成部材は、 一方の該連通路形成部材に接続するときに、 一方 の該連通路形成部材の前記閉塞部材を前記円筒部材内部に移動させる閉塞部材移 動手段を備える請求項 1〜 7のいずれかに記載の試験試料調製装置。  The other communicating path forming member includes a closing member moving means for moving the closing member of the one communicating path forming member into the cylindrical member when connected to the one communicating path forming member. The test sample preparation apparatus according to any one of 1 to 7.
1 0 . 互いに接続された 1組の前記連通路形成部材は、 互いに対向する端面に 設けられた端面部材連通孔をもつ 2つの端面部材と、 該端面部材の間であって該 端面部材の該端面に沿って移動可能に介設され、 且つ、 該 2つの端面部材の該端 面部材連通孔の間を連通させる連通孔が形成された連通切り替え部材と、 該連通 切り替え部材の移動に追随し、 該 2つの端面部材の間から該連通切り替え部材を 引き抜いたときに該端面部材連通孔に密着して閉塞する薄膜状のシール部材と、 を備える請求項 1〜 7のいずれかに記載の試験試料調製装置。 1 0. One set of the communication path forming members connected to each other includes two end surface members having end surface member communication holes provided on opposite end surfaces, and between the end surface members and the end surface members. A communication switching member provided movably along the end surface and having a communication hole communicating between the end surface member communication holes of the two end surface members; and following the movement of the communication switching member A thin-film seal member that closes and closes the end surface member communication hole when the communication switching member is pulled out from between the two end surface members; A test sample preparation apparatus according to any one of claims 1 to 7.
1 1 . 互いに接続される 1組の前記連通路形成部材のうち、  1 1. Of the set of communication path forming members connected to each other,
一方の該連通路形成部材は、弹性材料により端面に形成された密着部材を備え、 他方の該連通路形成部材は、一方の該連通路形成部材の該密着部材を突き刺して、 連通状態にする管である針状部材を備える請求項 1〜 7のいずれかに記載の試験 試料調製装置。  One of the communication path forming members includes a close contact member formed on an end surface of a coasting material, and the other communication path forming member pierces the close contact member of one of the communication path forming members to be in a communication state. The test sample preparation apparatus according to any one of claims 1 to 7, further comprising a needle-like member that is a tube.
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GB2590434A (en) * 2019-12-17 2021-06-30 Oribiotech Ltd An apparatus
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