EP1984729A1 - Procédé et dispositif d'aspiration d'un volume, notamment de prélèvement d'un échantillon aux fins d'analyse à l'aide d'un dispositif de chromatographie en phase liquide - Google Patents

Procédé et dispositif d'aspiration d'un volume, notamment de prélèvement d'un échantillon aux fins d'analyse à l'aide d'un dispositif de chromatographie en phase liquide

Info

Publication number
EP1984729A1
EP1984729A1 EP07702420A EP07702420A EP1984729A1 EP 1984729 A1 EP1984729 A1 EP 1984729A1 EP 07702420 A EP07702420 A EP 07702420A EP 07702420 A EP07702420 A EP 07702420A EP 1984729 A1 EP1984729 A1 EP 1984729A1
Authority
EP
European Patent Office
Prior art keywords
liquid
volume
needle
container
flexible material
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP07702420A
Other languages
German (de)
English (en)
Inventor
Hermann Hochgraeber
Michael Hene
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dionex Softron GmbH
Original Assignee
Dionex Softron GmbH
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 Dionex Softron GmbH filed Critical Dionex Softron GmbH
Publication of EP1984729A1 publication Critical patent/EP1984729A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1095—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers
    • G01N35/1097—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers characterised by the valves
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/18—Injection using a septum or microsyringe
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/24—Automatic injection systems
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
    • G01N35/1011—Control of the position or alignment of the transfer device
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1079—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices with means for piercing stoppers or septums
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • B01L3/5085—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates
    • B01L3/50853—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above for multiple samples, e.g. microtitration plates with covers or lids

Definitions

  • Method and device for aspirating a volume of liquid in particular for taking a sample for analysis by means of a
  • the invention relates to a method for aspirating a liquid volume, in particular for taking a sample for analysis by means of a liquid chromatography device, having the features of the preamble of claim 1. Furthermore, the invention relates to a device for carrying out the method according to claim 6.
  • HPLC High Performance Liquid Chromatography
  • Sampler used the samples, i. take a defined volume of liquid, one at a time, from a number of sample containers and feed them in turn to the analytical system.
  • Such samplers are known, for example, from US Pat. Nos. 4,242,909 and 4,713,974.
  • FIG. 1 shows a simplified, schematic representation of the essential components of a known sampler.
  • the liquid flow delivered by a pump enters the sampler, passes through a 6-port switching valve 2 and leaves the sampler via an output capillary 5.
  • the samples to be analyzed are in sample containers 7 and can use a sampling needle or Sample needle 6 are removed.
  • a schematically illustrated receiving unit 10 for the sample container 7 is provided.
  • the receiving unit may comprise a drive for positioning the individual sample containers 7 relative to the removal needle 6 in a plane substantially perpendicular to the longitudinal axis of the removal needle 6 and a mechanism suitable for this purpose. This alternative is indicated in Fig. 1 by the dashed arrow between a drive unit 12 for controlling the drive of the receiving unit 10.
  • the drive unit 12 can, as shown in Fig. 1, also drive a non-illustrated drive for the axial positioning of the removal needle 6 to allow an axial relative movement between the sample containers 7 and the withdrawal needle 6 to.
  • the relative movements that can be achieved by these two drives between the sample containers 7 or the receiving unit 10 and the withdrawal needle 6 in the direction of the longitudinal axis of the withdrawal needle 6 and in a plane (or direction) substantially perpendicular thereto are indicated in FIG. 1 by arrows I and II ,
  • the removal needle 6 can initially over any
  • Sample container 7 are positioned and then dipped or inserted into this to remove the respective sample.
  • the realization of the relative movements between the receiving unit 10 and the removal needle 6 can of course also be such that only the removal needle 6 or only the receiving unit 10 by means of suitable, controllable drives in the axial direction and in the plane perpendicular thereto is movable. In any case, at least two axes of movement are required to approach a plurality of sample containers 7 individually and to be able to immerse the withdrawal needle 6 into them.
  • the switching valve 2 has two switching positions: The position shown in FIG. 1 is referred to below as position 1-2, in each case the ports 1 are connected to 2, 3 to 4 and 5 to 6. The second position is referred to as position 6-1, wherein the ports 2 with 3, 4 with 5 and 6 are connected to 1. In position 1-2 is the
  • Input capillary 1 is connected directly to the output capillary 5. Furthermore, the metering syringe 4, the sample loop 3, the connecting capillary 8 and the removal needle 6 are connected in series. Initially, the switching valve 2 is in position 6-1, ie a metering syringe 4 is connected directly to the withdrawal needle 6 via a connecting capillary 8. In this case, the liquid stream arriving via the input capillary 1 is conducted via a sample loop 3 to an output capillary 5. While the Entnalimenadel 6 is immersed in a sample container 7, by suction by means of the metering syringe 4 which may also be formed controllable by the drive unit 12, a defined volume of liquid from the respective sample container 7 are removed.
  • injection The introduction of the sample into the liquid stream is referred to as injection.
  • the samples to be examined can be injected in any order.
  • the closure is usually made of a soft, elastic material and is referred to as a septum.
  • a septum is described, for example, in US Pat. No. 6,752,965 and has the advantage that it can simply be pierced by sampling needle 6 for sampling purposes and then largely self-sealed again. An elaborate mechanism for opening and closing the sample container is therefore unnecessary.
  • FIG. 2 shows two examples of such sealed sample containers.
  • FIG. 2 a shows a single sample container 7 for receiving a single sample liquid.
  • a receiving unit 10 according to FIG. 1 a plurality of such individual sample containers
  • a septum 71 is held by a cap 72, which has a breach in the middle, which leaves the septum 71 free.
  • the septum 71 can thus be pierced by the removal needle 6 in the region of the opening of the cap 72.
  • multiple sample containers 75 according to FIG. 2b so-called well plates, are increasingly used, in which depressions (so-called wells) 751 are provided for receiving the individual sample liquids.
  • the closure takes place in this case via a dimpled mat or stud plate 76, the studs 761 are each pressed into a recess 751 and close the opening of the respective recess.
  • Both the septum 71 and the dimpled mat 76 are made of an elastic material.
  • the sampling needle 6 pierces the septum 7 or the respective nub 761.
  • the elastic material is designed so that the sampling needle 6 is substantially tightly enclosed, as long as it is in the sample container 7 or in a recess 751. During the suction process, therefore, no ambient air can flow in for the sample volume removed, ie. it forms a negative pressure in the sample container. This is the stronger, the more full the sample container was at the beginning or the lower the trapped gas volume and the more sample liquid was sucked.
  • Another solution of the prior art is to greatly reduce the sampling rate of sampling. As a result, the risk of gas bubble formation is greatly reduced because air can flow through the ever-present small leaks between the needle and septum or septum and sample container.
  • solutions are known in which a pressure compensation is made possible by a special design of the sampling needle. These solutions either contain an additional ventilation channel in the sampling needle itself, or the sampling needle is shaped to allow access of air at the point where the sampling needle pierces the septum.
  • Object of the present invention is therefore to provide a method for aspirating a volume of liquid, in particular for taking a sample for analysis by means of a liquid chromatography device, in which the emergence of a
  • Negative pressure in the sample container is avoided during the sample aspiration without having to accept any restrictions with regard to the fill level of the sample container, the amount of sample sucked in or the suction rate.
  • the solution according to the invention should not have any undesired side effects such as increased wear of the septa or increased sample carryover.
  • the invention has the object to provide a device for carrying out the method.
  • the invention is based on the recognition that a significant negative pressure in the sample container can not even arise if, during the intake of the sample container
  • the invention is based on the consideration that the sealing effect of the septum during the Probenansaugung based on its elasticity and that this elasticity can be used to cancel the sealing effect at least temporarily and to allow a pressure equalization between the interior of the sample container and the environment.
  • the extraction needle and sample container being moved by a small amount relative to each other after piercing the flexible material (the septum), that is, while the sampling needle is in the sample container, the hole in the septum will become somewhat displaced by the sampling needle with a suitable choice of movement expanded. This ensures that in addition to the sampling needle air can enter the sample container and thus takes place a pressure equalization. Consequently, the Even large volumes of sample no longer suck to form a negative pressure in the sample container and the formation of gas bubbles is avoided.
  • the container and the removal needle are moved relative to one another in a direction substantially perpendicular to the longitudinal axis of the removal needle.
  • Such a movement can be realized in known sample dispensers with the already existing hardware. To realize only the control of the drives or the drives must be adjusted, but this is mainly possible by simple software or firmware changes.
  • the pressure compensation by the execution of the relative movement is only possible when a predetermined threshold for the absolute amount of the differential pressure between the container volume and the environment is present or detected.
  • the pressure compensation can be made possible by the execution of the relative movement only after a predetermined period of time after the start of the suction of the liquid volume or after the suction of a predetermined partial volume.
  • a device according to the invention for sucking in a liquid volume in particular for removing and supplying a sample to a liquid chromatography device, can only differ from known devices in that the control unit controls the drive or drives for moving the removal needle and the receiving unit for the sample container or containers are so is formed, that after the insertion of a relative movement between the receiving unit and withdrawal needle is executable such that a pressure equalization between the container interior and the environment is made possible.
  • control unit as is customary in practice, has a microprocessor circuit and a control software
  • the solution according to the present invention can be integrated into an existing device in a simple and cost-effective manner as part of a software or firmware change.
  • Figure 1 is a schematic representation of the essential for understanding the invention components of a sample dispenser for a liquid chromatography apparatus.
  • Figure 2 is a schematic representation of a single sample container (Figure 2a) and a multiple sample container (Figure 2b) for liquid chromatography;
  • FIG 3 is a schematic cross section through a septum piercing removal needle.
  • FIG. 4 shows a schematic side view of a single sample container accommodated in a receiving unit
  • Fig. 5b is a chromatogram in the case of no gas bubbles containing sample liquid.
  • Fig. 3 shows a greatly enlarged view in plan view of a schematic cross section through the withdrawal needle 6 in the region of a septum 71 of a closure of a sample container 7 or 75, in which the removal needle 6 is inserted for removing a sample volume or liquid volume. 3 shows the state that results when, after piercing the removal needle in the flexible
  • the existing hardware of the known per se sampler shown in Fig. 1 can be used, since this is designed to approach several different sample containers and thus allows a movement perpendicular to the axis of the withdrawal needle 6.
  • the predetermined volume of liquid can be sucked in without gas bubbles, without any restrictions with regard to the fill level of the sample containers, the intake volume or the intake speed.
  • the suction rate is limited only by the flow resistance of the fluidic components involved.
  • the inventive method for any, even existing sampler and septa can be applied without a significant additional expense arises. Only the control software or firmware of the autosampler must be adjusted so that the shift is executed at the right time.
  • sampling needle does not have sufficient stability, it can be simple
  • the displacement must be such that a sufficiently large opening 9 can be achieved. In this case, an unnecessarily strong bending of the removal needle 6 should be avoided. Therefore, the displacement must be optimized taking into account the influencing factors described below.
  • the septum 71 or a nub 761 of a dimpled mat 76 initially deforms over a large area due to the displacement, before an opening 9 is formed at all. This must be taken into account when defining the displacement path. In addition, it must be taken into consideration that individual sample containers 7 or multiple sample containers 75 (corrugated plates) usually have play in their holder of the receiving unit 10, so that they can deflect or tilt away due to the displacement. Furthermore, the force exerted on the extraction needle 6 results in bending of the needle.
  • sampling needles, sample containers and septa shifts in the order of 1 to 2 mm are usually appropriate.
  • smaller or larger displacements in the range 0.1 mm to 5 mm may be required.
  • the pressure equalization does not necessarily have to be made possible before the start of the liquid volume suction process. Because before the start of the suction process, the sampling needle 6 pierces the septum 71 and the nub 761. In doing so, the septum 71 or the nub 761 bends downwards. Because of the friction between the extraction needle 6 and septum 71 or nub 761 this deflection remains even after the piercing and causes due to the reduction of the interior of the container an overpressure. The volume displaced by the removal needle 6 likewise leads to overpressure. This overpressure may well be desirable, as it facilitates the suction of the liquid volume.
  • opening 9 would lead to premature degradation of this pressure.
  • volume was aspirated, that the pressure is already reduced.
  • the effectiveness of the method according to the invention was checked by means of chromatographic measurements. If negative pressure problems or gas bubbles arise during the aspiration of the sample, this initially leads to a change in the injected sample quantity and thus the chromatographic peak areas, in the case of larger bubbles to severely falsified, non-evaluable chromatograms.
  • Figure 5a shows the chromatograms of eleven consecutive measurements each without allowing pressure equalization. There are sometimes very different signal curves, indicating the formation of gas bubbles and sucked air and their injection. Such measurement results would be useless for the current automatic evaluation.
  • Fig. 5b also shows eleven chromatograms taken under identical conditions as in Fig. 5a, but with pressure equalization as described above.
  • the curves obtained now correspond to the expected course and are all exactly to each other. As a result, very good chromatographic reproducibility and measurement accuracy are achieved.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)

Abstract

L'invention concerne un procédé d'aspiration d'un volume de liquide, notamment de prélèvement d'un échantillon aux fins d'analyse à l'aide d'un dispositif de chromatographie en phase liquide. Le liquide contenant le volume de liquide à aspirer se trouve dans un contenant (7, 75) fermé par un couvercle (72, 71; 76, 761) qui est constitué, au moins dans une zone partielle, d'un matériau flexible apte à être transpercé par une aiguille de prélèvement. Pour procéder à l'aspiration d'un volume de liquide défini, on pique l'aiguille de prélèvement (6) dans la zone partielle de matériau flexible jusqu'à ce que l'orifice d'aspiration de l'aiguille de prélèvement soit immergé à une profondeur suffisante dans le liquide, un volume de liquide défini étant aspiré. L'invention vise à éviter que le prélèvement du volume de liquide ne génère un vide partiel dans le contenant (7, 75). A cet effet, un mouvement relatif est réalisé entre l'aiguille de prélèvement (6) et le contenant (7, 75) dans une direction sensiblement perpendiculaire à l'axe longitudinal de l'aiguille de prélèvement (6) de telle façon que l'orifice (9) réalisé par piquage dans le matériau flexible du couvercle (72, 71; 76, 761) soit agrandi afin de permettre, entre la paroi externe de l'aiguille de prélèvement (6) et la paroi interne de l'orifice (9), une compensation de pression complète ou partielle entre le volume du contenant et l'environnement.
EP07702420A 2006-02-16 2007-02-02 Procédé et dispositif d'aspiration d'un volume, notamment de prélèvement d'un échantillon aux fins d'analyse à l'aide d'un dispositif de chromatographie en phase liquide Withdrawn EP1984729A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006007542A DE102006007542B3 (de) 2006-02-16 2006-02-16 Verfahren und Vorrichtung zum Ansaugen eines Flüssigkeitsvolumens, insbesondere zur Entnahme einer Probe zur Analyse mittels einer Flüssigkeitschromatographievorrichtung
PCT/DE2007/000190 WO2007093150A1 (fr) 2006-02-16 2007-02-02 Procédé et dispositif d'aspiration d'un volume, notamment de prélèvement d'un échantillon aux fins d'analyse à l'aide d'un dispositif de chromatographie en phase liquide

Publications (1)

Publication Number Publication Date
EP1984729A1 true EP1984729A1 (fr) 2008-10-29

Family

ID=38161979

Family Applications (1)

Application Number Title Priority Date Filing Date
EP07702420A Withdrawn EP1984729A1 (fr) 2006-02-16 2007-02-02 Procédé et dispositif d'aspiration d'un volume, notamment de prélèvement d'un échantillon aux fins d'analyse à l'aide d'un dispositif de chromatographie en phase liquide

Country Status (7)

Country Link
US (1) US20090044607A1 (fr)
EP (1) EP1984729A1 (fr)
JP (1) JP2009526974A (fr)
AU (1) AU2007214898A1 (fr)
CA (1) CA2642293A1 (fr)
DE (1) DE102006007542B3 (fr)
WO (1) WO2007093150A1 (fr)

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CN113104331A (zh) * 2021-03-25 2021-07-13 武汉佰美斯医疗科技有限公司 一种管道封装液体的取出方法

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WO2010119801A1 (fr) * 2009-04-16 2010-10-21 株式会社島津製作所 Système de chromatographie liquide
JP5410254B2 (ja) * 2009-12-03 2014-02-05 安井器械株式会社 検体検査の検査前処理方法と装置
JP4936235B2 (ja) * 2009-12-21 2012-05-23 株式会社日立プラントテクノロジー 発光測定装置の試薬開封機構および試薬開封機構における開封針制御方法
CN101881706B (zh) 2010-07-05 2014-04-02 深圳迈瑞生物医疗电子股份有限公司 一种采样设备及方法
JP2012237557A (ja) * 2011-05-09 2012-12-06 Shimadzu Corp 液体試料採取装置及び液体試料採取方法
JP6318595B2 (ja) * 2013-12-12 2018-05-09 東ソー株式会社 試料吸引装置
DE102014109631B3 (de) 2014-07-09 2015-05-21 Dionex Softron Gmbh Probenentnahmeeinheit
CN106482985B (zh) * 2016-11-11 2023-03-14 长安大学 基于负压取样法的自动出针式多样本气液取样器
EP3555634B1 (fr) * 2016-12-16 2023-09-06 Ventana Medical Systems, Inc. Réduction de résidus de pipettes
CN107192579A (zh) * 2017-05-11 2017-09-22 赵连文 一种多功能用于医学检验提取器
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CN113104331A (zh) * 2021-03-25 2021-07-13 武汉佰美斯医疗科技有限公司 一种管道封装液体的取出方法

Also Published As

Publication number Publication date
JP2009526974A (ja) 2009-07-23
CA2642293A1 (fr) 2007-08-23
WO2007093150A1 (fr) 2007-08-23
DE102006007542B3 (de) 2007-09-20
US20090044607A1 (en) 2009-02-19
AU2007214898A1 (en) 2007-08-23

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