EP0611596A1 - Système pour la préparation de liquides - Google Patents

Système pour la préparation de liquides Download PDF

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Publication number
EP0611596A1
EP0611596A1 EP94101748A EP94101748A EP0611596A1 EP 0611596 A1 EP0611596 A1 EP 0611596A1 EP 94101748 A EP94101748 A EP 94101748A EP 94101748 A EP94101748 A EP 94101748A EP 0611596 A1 EP0611596 A1 EP 0611596A1
Authority
EP
European Patent Office
Prior art keywords
vessel
solid
desiccant
liquid
liquid phase
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.)
Granted
Application number
EP94101748A
Other languages
German (de)
English (en)
Other versions
EP0611596B1 (fr
Inventor
Herbert Buschek
Michael Kühnl
Roland Ihrig
Klaus Dr. Erler
Maria Dr. Cully
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.)
Roche Diagnostics GmbH
Original Assignee
Roche Diagnostics GmbH
Boehringer Mannheim 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 Roche Diagnostics GmbH, Boehringer Mannheim GmbH filed Critical Roche Diagnostics GmbH
Publication of EP0611596A1 publication Critical patent/EP0611596A1/fr
Application granted granted Critical
Publication of EP0611596B1 publication Critical patent/EP0611596B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
    • B01L3/508—Containers for the purpose of retaining a material to be analysed, e.g. test tubes rigid containers not provided for above
    • 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
    • B01L3/5082—Test tubes per se
    • B01L3/50825—Closing or opening means, corks, bungs

Definitions

  • the invention relates to a system for preparing liquids from at least one solid and at least one liquid phase, the system consisting of a storage vessel with the solid and a drying chamber with a desiccant.
  • the invention also relates to a method for producing a solution, suspension or emulsion using the system according to the invention.
  • the process includes the steps of storing a solid in the system, adding a liquid phase to the solid, and mixing to produce a solution, suspension or emulsion.
  • the system is used to prepare reagent solutions.
  • a common problem in laboratories is the preparation of solutions from liquids and moisture-sensitive solids. Many solids have a limited shelf life in the presence of water vapor because they decompose. The occurrence of this problem ranges from everyday examples, such as. B. the preparation of food from dry powder, the preparation of solutions in the chemical laboratory, up to clinical analysis solutions. In the latter case in particular, preparation of the solution from a solid and a liquid component is necessary shortly before use if the finished analytical solution has a limited shelf life.
  • the existing problem is solved in that the moisture-sensitive solid is either pre-dried and packaged in a water vapor-tight manner or is packed together with hygroscopic substances for drying and keeping dry. To prepare the solution, a certain amount of the substance is weighed out and dissolved in a measured amount of liquid.
  • the method is particularly imperfect for analytical solutions because the quantitative transfer of the solid into a vessel, the addition of a precisely defined amount of solvent and complete dissolution are difficult. Not only trained personnel are required for this process, but also complex laboratory equipment.
  • test kits In so-called test kits, the user takes over the preparation of the liquid by preparing the analytical solution from the portioned, ie already weighed, solids by adding liquid according to a rule given by the manufacturer of the kit. Stirrers or mixers can reduce the solids from the user. In these cases, however, a transfer of solid matter to a vessel is necessary for dissolution. It follows from this that a defined amount of solid in the form of tablets, powders or granules has to be introduced into a vessel in order to produce a solution of a defined concentration.
  • a known reagent storage system (DE-40 39 580)
  • the reagent is transferred from a special container into a mixing vessel by opening a chamber in which the reagent is located when it is screwed onto the vessel. To prepare a solution of a precisely defined concentration, the chamber must be rinsed. This makes laboratory personnel or a complex flushing device necessary.
  • the object of the invention is to simplify the production of liquids from moisture-sensitive solids and liquids by providing a vessel suitable for drying and keeping dry.
  • the preparation of analysis solutions by untrained personnel, even under conditions of poor infrastructure, should be made easier.
  • the task is achieved with the system for the preparation of a liquid from at least one solid and at least one liquid phase by the combination a vessel which contains the at least one solid and has a volume which is sufficient to hold the at least one solid and the at least one liquid phase, a desiccant chamber containing a desiccant (TM) and a separating element, which closes the desiccant chamber, that the desiccant can exchange water vapor with the contents of the vessel at any time, but the direct contact of a liquid or solid content of the vessel with the desiccant is essentially impossible.
  • TM desiccant
  • separating element which closes the desiccant chamber
  • the solid of the solution to be prepared can be in various forms. These include powders, tablets, granules, pellets or freeze-dried lyophilisates.
  • a solution consisting of several substances can be prepared by using a solid consisting of several components. If the constituents in solution or in the presence of moisture are incompatible with one another, that is, if they then react with one another in an undesired manner, it is in many cases possible to store the substances together in a dry state without them reacting with one another.
  • the storage stability of the solid is increased by a drying chamber that keeps the moisture in the interior of the vessel low.
  • the presence of a desiccant in a chamber that can exchange water vapor with the interior of the vessel leads to a lowering of the water vapor partial pressure in the interior of the vessel. It is also possible to store solids which have residual moisture due to the manufacturing process in the system according to the invention for drying or to remove the residual moisture.
  • the liquid phase can consist of a pure substance (e.g. distilled water) or a mixture of several liquids.
  • the liquid phase can also, for. B. contain buffers, stabilizers or other solutes, so that the stability of the liquid produced is increased and its functioning is ensured.
  • the liquid phase is added to the solid in the vessel. This can be done either manually or automatically by a device. In cases where the liquid produced does not have to have an exact concentration, because a wide range of reagent concentrations leads to the same analysis results, the dimensioning of the liquid phase can, for. B. done by markings on the vessel wall. For example, enzymes can completely convert an analyte so that the result of the determination is largely independent of the enzyme concentration in the reagent.
  • a standard solution suitable for titration analysis on the other hand, it is necessary to add a defined amount of liquid phase, characterized by its volume or weight, to a defined amount of solids.
  • the solution is prepared by manual or mechanical mixing of the solid and the liquid phase. For a large number of analysis solutions, it is possible to standardize their preparation.
  • the liquid phase already contains further components, e.g. B. buffers and auxiliaries, so that one and the same liquid phase can always be used for many different analytical solutions.
  • the liquids produced from solid and liquid phase in the system according to the invention can be solutions, suspensions or emulsions.
  • an emulsion for the detection of the enzyme lipase can be prepared by adding water to a solid which contains the following substances: tris (hydroxymethyl) aminomethane (tris), sodium deoxycholate, CaCl2, triolein, colipase, NaN3.
  • the system includes a vessel and a drying chamber which are separated by a separating layer which prevents liquid from penetrating into the drying agent.
  • the interface therefore fulfills two contradictory conditions. On the one hand, it is permeable to water vapor and thus enables the transfer of water from the interior of the vessel into the drying chamber via the gas phase, on the other hand it has a barrier effect for water in the condensed phase. This simplifies the manufacturing process in that the solution can be prepared in the same vessel in which the moisture-sensitive solid was previously stored.
  • the solid is poured into the vessel during the manufacture of the system. In this case, the user does not need to transfer the solid into the vessel.
  • a particularly simple, safe and reliable handling is made possible by a preferred embodiment in which the solid is in a vessel which is large enough to take up the resulting solution.
  • This vessel has a closure, e.g. B. a stopper or a screw cap, on which a desiccant chamber is attached so that the desiccant it contains can absorb water vapor from the interior of the vessel when the vessel is closed.
  • the Drying chamber both serve to dry and / or keep the solid dry, and can also be used as a closure in the preparation of liquids.
  • the filling of the vessel with liquid phase can be done manually or mechanically, the automatic filling of the vessel within an automatic analyzer being a preferred embodiment.
  • the vessel can be closed with the closure belonging to the system, or but another closure. Both manual and automated procedures are also possible in this process step.
  • the step of closing the vessel can be saved if there is no leakage of liquid from the vessel during the mixing. This can e.g. B. can be achieved by stirring or suitable pivoting of the vessel.
  • so-called magnetic stirrers are known, among other things, in which a mostly rod-shaped magnet is located within the vessel, which is set in motion by a magnetic field.
  • swivels are known, for example, for bacterial cultures, which mix the contents of a vessel without substances in the vessel escaping through an existing opening at the top of the vessel. If the mixing process is carried out with the vessel closed, the methods already mentioned are available. In addition, methods are possible in which the vessel can assume any position, as is usually the case with manual mixing. After the mixing process, the prepared liquid is present in the vessel. For this she can, for. B. by piercing the vessel with a cannula or by other devices provided in the vessel. Preferably, however, liquid is removed after the closure containing the desiccant has been removed through the opening in the vessel.
  • the storage vessel for the solid also serves as a vessel for mixing the solid with the liquid phase and can serve to store the prepared liquid without the desiccant chamber having to be closed or removed after the liquid phase has been added.
  • a further advantage of the system is that the seal containing the drying agent can be used both during storage of the solid and during storage of the prepared liquid and preferably even during the mixing of the solid with the liquid phase.
  • a preferred embodiment of the desiccant chamber is suitable due to its construction to close the vessel.
  • Such a desiccant chamber is referred to below as a desiccant plug.
  • the drying agent stopper (1) in FIG. 1 is closed off from the outside by a wall (2).
  • a wall (2) This can consist of a variety of materials, e.g. B. plastic, metal and cardboard.
  • the wall will consist of a plastic, since this material combines some advantageous properties.
  • Plastics of sufficient wall thickness, preferably greater than 0.5 mm have the property of separating the desiccant inside the stopper from the environment in such a way that moisture exchange between the environment and desiccant is possible to a small extent, but a significant consumption of the desiccant by external moisture is avoided.
  • the desiccant (14) is inside the stopper.
  • a suitable drying agent the substances known from the specialist literature, such as molecular sieves, silica gel, sodium sulfate, calcium sulfate, etc., are available.
  • a molecular sieve of the zeolite type suitable for the stated use is available from Grace GmbH under the name molecular sieve type 511.
  • the amount of desiccant used and thus the drying capacity must be such that, if desired, a possible mobile moisture content of the solid is absorbed and that moisture which penetrates from outside can be absorbed until the solution is prepared.
  • the amount of desiccant should be so small that when the liquid produced is stored in the preparation system there is no significant change in concentration due to the absorption of water by the desiccant from the solution.
  • preferred desiccant amounts in the range of a few grams and quantities of liquid in the range of deciliters, the error caused by the desiccant moves in a range acceptable for analytical solutions.
  • the liquid is used in an analytical apparatus soon after it has been prepared.
  • the vessel is placed in a place provided within the apparatus without a desiccant plug. In this case, the liquid is only in direct or indirect contact with the desiccant plug while it is being prepared.
  • the drying effect of the solution can therefore only be expected to a very small extent. The drying out effect can be prevented in all cases by exchanging the drying agent plug after the solid and liquid phase have been mixed with a closure without drying agent.
  • the separating element (6) which separates the desiccant and the interior of the vessel from one another, represents an essential aspect of the invention.
  • the material of the separating element is such that it is permeable to water vapor, but completely blocks finished reagent solutions.
  • special plastics have been developed that combine these two properties (e.g. EP-A-0 500 173).
  • other materials are also possible, such as. B. impregnated fabrics and cardboard.
  • cardboard with a surface tension is used which prevents liquid from penetrating into the drying agent chamber and penetrating the drying agent with liquid. Suitable cartons are sold, for example, by Buchmann GmbH under the names GC1 and GC2 or by Laakmann GmbH under the names UD2.
  • the water-repellent effect is primarily due to a Coating, the so-called line, which consists of pigments and synthetic binders.
  • the cardboard has a surface tension of less than 70 mN / m, the cardboard can no longer be wetted by water and penetration of water is in principle impossible, but water vapor is still permeable.
  • a separating element with a lower surface tension is also necessary to prevent the penetration of liquids.
  • the surface tension of the cardboard can be easily obtained with commercially available test inks from e.g. B. the company Arcotec heatntechnik GmbH can be determined.
  • FIG. 1 A possible arrangement of the separating element is shown in Figure 1.
  • the separating element (6) is fitted into a hollow pin (5) in such a way that the liquid does not pass from the interior of the vessel to the desiccant. In a preferred embodiment, this is achieved by the separating element (6) resting on the opening of the hollow pin (5) facing the interior of the vessel.
  • a flange (7) is mechanically connected to the hollow pin and is used to fasten the separating element (6) on the hollow pin (5).
  • the flanging (7) closes off the space formed from drying agent chamber (4) and separating element (6) against liquids. Any minor leaks are sealed by swelling the separating element in contact with water and filling the gaps.
  • Example 1 demonstrates the separating effect of the cardboard used against an aqueous reagent liquid even in the case of direct contact.
  • FIG. 2 shows vessels according to the invention arranged in a circle with desiccant plugs and in the middle two desiccant plugs with a volume of 2 or 4 ml for desiccant.
  • the materials of the vessels must be impermeable to water, but can be partially permeable to water vapor.
  • plastics are suitable, such as those used for the production of bottles for storing liquids.
  • wall thicknesses greater than 0.5 mm are preferred for reasons of mechanical stability and water vapor permeability.
  • the way of making the vessels e.g. B. injection molding or blow molding is not subject to any restriction, provided that a sufficient wall thickness can be guaranteed.
  • FIG. 3 shows the production of a liquid from a solid and a liquid.
  • the solid is in the container closed by the desiccant plug.
  • illustration B shows the addition of liquid to the solid.
  • the solid is mixed with the liquid phase in FIG. 3C by shaking.
  • the resulting reagent solution for determining GOT then had the following composition: Tris 27.8 mmol / l Tris HCL 58.4 mmol / l L-aspartate 254 mmol / l -Ketoglutarate 12.7 mmol / l NADH 0.19 mmol / l 2-chloroacetamide 10.7 mmol / l MDH 1200 U / l LDH 4390 U / l Polyvinyl pyrolidone approx. 0.1% by weight
  • the reagent solution for the determination of GPT had the following composition: Tris 15.9 mmol / l Tris ⁇ HCL 89.6 mmol / l L-alanine 530 mmol / l -Ketoglutarate 15.9 mmol / l NADH 0.19 mmol / l 2-chloroacetamide 10.7 mmol / l LDH 8900 U / l Polyvinyl pyrolidone approx. 0.1% by weight
  • the vessels were stored on the head for up to 24 hours, which is much more than the stress during normal use.
  • the screw caps were then unscrewed and the cardboard separating elements (cardboard UD2 from Laakmann GmbH) removed for inspection of the desiccant.
  • the desiccant was still dry, i.e. H. the blocking effect was given in all cases.
  • test results are shown in the following table: reference 8 h / head 16 h / head 24 h / head swing GOT reagent w [%] 100.00 99.87 99.87 99.41 99.74 NADH absorbance 1,370 1,392 1,397 1,430 1,373 GPT reagent w [%] 100.00 99.92 99.44 99.12 99.76 NADH absorbance 1,392 1,400 1,412 1,406 1,390
  • the measured values show that the functionality of the reagent and the active substance content are only insignificantly influenced by the presence of the desiccant plug, even under extreme loads.
  • the solid which can be used for the preparation of reagent liquid for the determination of GPT, contained in 100 g of granules: Tris 2.72 g Tris ⁇ HCL 20.06 g L-alanine 67.07 g -Ketoglutarate 5.09 g NADH 1.34 g 2-chloroacetamide 1.42 g LDH approx. 0.34 g Polyvinyl pyrolidone approx.1.93 g
  • the example “GOT” additionally shows that only the stability-critical mobile moisture is selectively removed and the stability-uncritical immobile crystal water content remains unaffected.
  • the system was kept in a room climate during the redrying phase and the water content was determined periodically using the Karl Fischer method.
  • FIG. 4 shows the dependence of the water content (f) as a function of the storage time (t) in days in the system.

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Hematology (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Packages (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Photographic Developing Apparatuses (AREA)
  • Investigating Or Analysing Biological Materials (AREA)
EP94101748A 1993-02-13 1994-02-05 Système pour la préparation de liquides Expired - Lifetime EP0611596B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4304450 1993-02-13
DE4304450A DE4304450A1 (de) 1993-02-13 1993-02-13 System zur Zubereitung von Flüssigkeiten

Publications (2)

Publication Number Publication Date
EP0611596A1 true EP0611596A1 (fr) 1994-08-24
EP0611596B1 EP0611596B1 (fr) 1998-01-07

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EP94101748A Expired - Lifetime EP0611596B1 (fr) 1993-02-13 1994-02-05 Système pour la préparation de liquides

Country Status (7)

Country Link
US (1) US6274304B1 (fr)
EP (1) EP0611596B1 (fr)
JP (1) JP2558434B2 (fr)
AT (1) ATE161755T1 (fr)
CA (1) CA2115379C (fr)
DE (2) DE4304450A1 (fr)
ES (1) ES2113563T3 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE29513987U1 (de) * 1995-08-18 1995-10-26 Friedrich Sanner GmbH & Co KG Spritzgußwerk, 64625 Bensheim Behälter-Verschluß mit Trockenstoffkammer
WO1997029846A1 (fr) * 1996-02-13 1997-08-21 Aalto Scientific, Ltd. Dispositifs de pipettage precharges avec des matieres normalisees pour echantillons temoins
DE19850934C2 (de) * 1998-11-05 2001-07-12 Lange Gmbh Dr Bruno Verschlußelement zum Verschließen, Aufbewahren und Einbringen von Reagenzien und/oder Hilfsstoffen in einen Reaktionsbehälter
EP2175999B1 (fr) 2007-06-21 2017-01-04 Gen-Probe Incorporated Réceptacles pour l'exécution de procédés
DE102007051968A1 (de) * 2007-10-31 2009-05-07 Fischerwerke Gmbh & Co. Kg Mehrkomponenten-Kartusche
US9103749B2 (en) * 2012-10-11 2015-08-11 Fast Forward Forensics, LLC Biological sample collection apparatus
WO2015031827A1 (fr) * 2013-09-02 2015-03-05 Moxiyo, LLC Compositions d'absorption d'oxygène et conservation de marchandises périssables sensibles à l'oxygène
WO2017210218A1 (fr) * 2016-05-31 2017-12-07 Siscapa Assay Technologies, Inc. Dispositif et procédé de collecte d'échantillon

Citations (4)

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FR2341852A1 (fr) * 1976-02-19 1977-09-16 Sages Nouveau tube d'emballage
US4119407A (en) * 1976-03-08 1978-10-10 Bio-Dynamics, Inc. Cuvette with reagent release means
DE4039580A1 (de) * 1990-12-12 1992-06-17 Boehringer Mannheim Gmbh Reagenzbevorratungssystem und mehrfunktionsbehaelter fuer trockene reagenzkomponenten und anderes schuettgut
US5128104A (en) * 1987-04-27 1992-07-07 Murphy Harold R Cuvette for automated testing machine

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US1655248A (en) * 1924-08-16 1928-01-03 Panay Horizontal Show Jar Comp Moisture-regulating device
US2317882A (en) * 1940-05-31 1943-04-27 Charles F Boesel Absorbent closure cap for receptacles containing dry medicinal materials and the like
US2446361A (en) * 1945-07-09 1948-08-03 Herbert B Clibbon Moisture vapor indicator for packaged goods
US2487620A (en) * 1946-03-08 1949-11-08 Waller Fred Desiccator
US2548168A (en) * 1949-01-04 1951-04-10 Luce Mfg Company Food receptacle with desiccant
US2676078A (en) * 1950-07-21 1954-04-20 James Howard Young Canister
US3732627A (en) * 1970-11-23 1973-05-15 R Wertheim Removal of a liquid phase from a material
US3990872A (en) * 1974-11-06 1976-11-09 Multiform Desiccant Products, Inc. Adsorbent package
JPS5836505B2 (ja) * 1980-06-30 1983-08-09 富士通株式会社 半導体記憶装置の製造方法
US4374139A (en) * 1981-11-09 1983-02-15 Hoffmann-La Roche Inc. Levorotatory N-substituted acylmorphinans useful as analgesic agents
US4350508A (en) * 1981-12-21 1982-09-21 Santoro Dario S Desiccant cap
US4545492A (en) * 1982-09-30 1985-10-08 Firestone Raymond A Device for maintaining dry conditions in vessels
DE3715938A1 (de) * 1987-05-13 1988-11-24 Boehringer Mannheim Gmbh Behaelter fuer teststreifen

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2341852A1 (fr) * 1976-02-19 1977-09-16 Sages Nouveau tube d'emballage
US4119407A (en) * 1976-03-08 1978-10-10 Bio-Dynamics, Inc. Cuvette with reagent release means
US5128104A (en) * 1987-04-27 1992-07-07 Murphy Harold R Cuvette for automated testing machine
DE4039580A1 (de) * 1990-12-12 1992-06-17 Boehringer Mannheim Gmbh Reagenzbevorratungssystem und mehrfunktionsbehaelter fuer trockene reagenzkomponenten und anderes schuettgut

Also Published As

Publication number Publication date
JPH06247476A (ja) 1994-09-06
ES2113563T3 (es) 1998-05-01
ATE161755T1 (de) 1998-01-15
DE59404909D1 (de) 1998-02-12
JP2558434B2 (ja) 1996-11-27
DE4304450A1 (de) 1994-08-18
EP0611596B1 (fr) 1998-01-07
CA2115379A1 (fr) 1994-08-14
CA2115379C (fr) 2000-10-17
US6274304B1 (en) 2001-08-14

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