WO2013044331A1 - Dispositif pour l'extraction en phase solide de type "collecteur" avec chambre à vide, valves pour commande par vide et valves adaptées pour commande par pompe péristaltique - Google Patents

Dispositif pour l'extraction en phase solide de type "collecteur" avec chambre à vide, valves pour commande par vide et valves adaptées pour commande par pompe péristaltique Download PDF

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Publication number
WO2013044331A1
WO2013044331A1 PCT/BR2011/000463 BR2011000463W WO2013044331A1 WO 2013044331 A1 WO2013044331 A1 WO 2013044331A1 BR 2011000463 W BR2011000463 W BR 2011000463W WO 2013044331 A1 WO2013044331 A1 WO 2013044331A1
Authority
WO
WIPO (PCT)
Prior art keywords
vacuum
phase extraction
solid phase
peristaltic pump
valves
Prior art date
Application number
PCT/BR2011/000463
Other languages
English (en)
Portuguese (pt)
Inventor
Ricardo Mathias ORLANDO
Susanne Rath
Jarbas José Rodrigues ROHWEDDER
Original Assignee
Universidade Estadual De Campinas - Unicamp
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 Universidade Estadual De Campinas - Unicamp filed Critical Universidade Estadual De Campinas - Unicamp
Publication of WO2013044331A1 publication Critical patent/WO2013044331A1/fr

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40Concentrating samples
    • G01N1/4055Concentrating samples by solubility techniques
    • G01N2001/4061Solvent extraction
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/02Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations
    • G01N35/028Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a plurality of sample containers moved by a conveyor system past one or more treatment or analysis stations having reaction cells in the form of microtitration plates

Definitions

  • the present Utility Model patent relates to a manifold device for solid phase extraction which allows simultaneous and individualized extraction of various extraction cartridges and discs.
  • This equipment features a set of valves that are connected and controlled to a vacuum line and another set of which are connected and controlled to a peristaltic pump.
  • This solid phase extraction system is primarily intended for chemical, pharmaceutical, food and biotechnology laboratories and industries.
  • Solid phase extraction with cartridges and discs represents a large portion of the sample preparation procedures due to the peculiar advantages of this technique (Spears, 2004).
  • Standard SPE procedures require four to five steps in which liquid sample and other solvents pass through the sorbent filling the inside of the cartridge or disc.
  • This system consists basically of three main parts: a vacuum chamber; a valve cap to couple the cartridges and discs and a crate to support the tubes receiving the eluate of interest.
  • a vacuum chamber a vacuum chamber
  • a valve cap to couple the cartridges and discs and a crate to support the tubes receiving the eluate of interest.
  • solutions are percolated through the cartridge or discs to prepare them to receive the sample (conditioning step) as well as to remove the interferents present in the matrix (wash step). These solutions are generally not of interest to the final analysis and are therefore discarded. In the patented Wachob and Rightnour manifold these discarded solutions are necessarily directed into the vacuum chamber. Manifolds operating in this manner have four operational limitations.
  • the first is the need to exchange the vials within the vacuum chamber to receive the eluate of interest.
  • the second limitation is that the maximum volume of solution that can be percolated by the cartridges and disks should not exceed the volume of the vacuum chamber unless an additional stop is made for removal of the volume present within the vacuum chamber.
  • the third limitation is that since the vacuum chamber is a common part and shared with all system cover valves, the cartridge or disc that finishes the elution step faster than the others needs to wait for the slowest cartridge or disc to vacuum is turned off and the lid can be opened.
  • the fourth and last limitation is that the use of vacuum as a percolation device does not allow precise control of the solution flow in the cartridge or disk and, in SPE, the use of controlled flow rates is essential for maximum extraction and repeatability. suitable in extraction replicates.
  • peristaltic pump for a manifold system
  • US4079009 1978
  • the peristaltic pump operated in positive pressure mode which can lead to problems associated with compressible air trapped in the cartridge.
  • both conditioning and wash and eluate solutions are directed by a single path to the collection bottle, requiring the exchange of this collection collect the eluate of interest.
  • this invention does not disclose the use of an integrated vacuum system which is critical for use both for drying the cartridge after washing and for removing the remaining solvent trapped in the sorbent during the elution step.
  • Another developed device describes a manifold for SPE employing membranes (Patent 5529694, 1996).
  • the disclosed invention utilizes a valve system for directing vacuum to two different vials which avoids stopping to change vials, however the invention does not allow multiple simultaneous extractions nor the use of conventional SPE cartridges in their various sizes. In addition, its use is not compatible with a peristaltic pump to precisely control flow.
  • Patent DE202006013644 In 2006 another invention developed for SPE employing cartridges and discs was described (Patent DE202006013644).
  • the invention is basically a vacuum chamber subdivided into two compartments separated by a wall. This configuration allows the vacuum chamber to be emptied without stopping the system.
  • the proposed system requires all coupled cartridges to be in the same step as the procedure, does not allow the eluate manifolds of interest to be positioned prior to completion of the predecessor wash and conditioning steps, and is not capable of coupling either. peristaltic pump for precise flow control.
  • the funnel inlet should be at least larger than the largest commercially available cartridge requiring it to be inconveniently large.
  • this invention describes the possibility of the system being coupled to a peristaltic pump to more accurately control the flow of percolated liquids.
  • both the discarded and the collected liquids for analysis pass through the individual central chamber which necessitates the periodic cleaning of the same and / or the need to stop the process to place a clean collecting tube that will receive the fraction or eluate. of interest.
  • Orlando and Rath (18090056725 and 18090056147) filed a patent for two new valve manifold devices for eluate control.
  • These systems allow control by peristaltic pump, but only during the conditioning, sample application and washing steps, while in the eluate collection step of interest the peristaltic pump cannot be applied.
  • both use a single glass main vacuum chamber during the elution of the fraction of interest.
  • This type of vacuum chamber in addition to the risk of implosion during vacuum application, requires the synchronization of steps to avoid unnecessary stops, which makes the procedure slower.
  • the inventions presented in 2009 also have the disadvantage of possible cross contamination by sample interferers since the eluates of the various steps necessarily share at least part of the path during extractions.
  • Orlando, Rath and Rowhedder in 201 1 also disclose a manifold model consisting of a set of independent valves and chambers that direct the discarded eluates into a container intended solely for this purpose.
  • the described system also allows larger volumes than the vacuum chamber to be percolated without the need to change the collecting container, and also that the optional flow control can be performed through a peristaltic pump coupled to the system to achieve better flow control and thus increase repeatability between extractions.
  • a second set of valves was used to avoid contamination of the sample application and washing step.
  • the system described herein comprises a single-line manifold into which a conventional manifold solid-phase extraction valve assembly and a conventional manifold valve assembly which have been tailored to their outlet and which are connected and connected are inserted. controlled by a peristaltic pump.
  • This new device is differentiated primarily by the restructuring of its form, which has brought advantages both in its use (equipment operation) and in its production process.
  • This utility model patent application refers to a solid phase manifold manifold device that allows for simultaneous and individualized extraction of various extraction cartridges and discs.
  • the equipment consists basically of:
  • the present invention further comprises the use of the system described for any solid phase extraction process whether or not coupled to a vacuum pump and / or a peristaltic pump.
  • Figure 1 shows the schematic representation of a conventional commercial manifold SPE system with cartridges and manifolds and their operation.
  • Figure 2 shows a schematic representation of the developed prototype of the invention based on the commercial manifold system.
  • Figure 3 shows a front view of the prototype of the invention developed with emphasis on the base with a horizontal vacuum channel (18) and the opening regions of the open and close valves (19).
  • Figure 4 shows a top view of the prototype of the invention developed with emphasis on the base with a horizontal vacuum channel (18) in addition to the socket with base (19) of the adapted valves.
  • Figure 5 shows a right side view of the prototype of the invention (26) developed with emphasis on the horizontal base fixing screws (20).
  • Figure 6 shows a view of the left side base (21) of the prototype of the invention developed with emphasis on the horizontal base fixing screws (20) in addition to the threaded coupler and spigot end (13).
  • Figure 7 shows the schematic representation of a conventional open and close manifold valve.
  • Figure 8 shows the schematic representation of an open and close valve with an adaptation (26) for coupling to peristaltic pump lines.
  • This utility model patent application refers to a solid phase extraction manifold device which allows simultaneous and individualized extraction of multiple extraction cartridges and disks.
  • This equipment features a set of valves that are connected and controlled to a vacuum line and another set of which are connected and controlled by a peristaltic pump.
  • the Utility Model utilizes two independent valve assemblies, one coupled to a vacuum line and one coupled to peristaltic pump tubing.
  • the valves of this invention are the same as those described for conventional manifolds and only receive an adaptation in case of coupling to the peristaltic pump tubing.
  • the eluate collection stage of interest is performed by employing manifolds coupled to the adapted caps that simultaneously fit the cartridges and the open-and-close valves.
  • This invention allows all steps of the extraction process to be performed either by vacuum pump or peristaltic pump.
  • This configuration represents a constructive simplification of all conventional systems, as well as a decrease in operating variables, which reduces errors and operator fatigue, makes the manifold smaller, lighter, easier to carry, more impact resistant and simpler cleaning.
  • valve fittings (16) f - at least one valve assembly adapted (17) for coupling to peristaltic pump pipes and positioned to one of the system bases;
  • g - at least two side bases (21) for engaging, supporting and stabilizing the system;
  • Cartridges or discs that may be employed in the solid phase extraction system of the invention are all those used in conventional manifold systems.
  • FIG. 1 Also shown in Figure 1 are some features of the operation of a conventional commercial manifold SPE system.
  • the liquids percolated through the cartridges (6) are directed vertically to the main vacuum chamber (7) through the use of gravity or with the aid of a vacuum pump coupled to the system at the vacuum inlet (8).
  • the maximum volume that can be percolated without interruption should not exceed the volume of the collecting vials (9) or the main vacuum chamber (10).
  • the system must be stopped to position clean collection vials that will collect the analytes of interest in the elution step.
  • Figure 2 shows the prototype developed based on the commercial manifold system with the horizontal base (11) containing a vacuum channel with vertical holes for fitting the conventional open and close valves (12). These two devices are used for coupling the cartridges during the conditioning, sample application and washing steps when vacuum control is performed. Also shown in this figure are the threaded coupler (13) and spigot end (14) for vacuum hose fitting and vacuum gauge (15). Also appear is the base with vertical holes (16) for fitting open-and-close valves adapted to fit pipelines with peristaltic pumps (17).
  • Figure 3 is a front view of the developed prototype of the invention (without the vacuum gauge) with emphasis on the base with a horizontal vacuum channel (18) and the locking regions of the open and close valves (19). This figure also shows the positions of the horizontal and lateral base fixing screws (20).
  • Figure 4 is a top view of the developed prototype of the invention (without the vacuum gauge) with emphasis on the base with a horizontal vacuum channel (18) inserted into the base and the locking regions of conventional open and close valves. and adapted (19). This figure also shows the positions of the horizontal and lateral base fixing screws (20).
  • Figure 5 is a front view of the right base of the prototype of the invention developed with emphasis on the base (21) and the position of the fixing screws (20). This base may further contain handles or holes (22) for ease of handling.
  • Figure 6 is a front view of the right base of the prototype of the invention developed with emphasis on the base (21), the position of the fixing screws (20), the hole for easy handling (22), the threaded coupler (13) ) and the spike terminal (14).
  • the holes for easy handling can be replaced by support handles.
  • Figure 7 is a front view of the conventional open and close valve. In this figure the cartridge nozzle engaging regions (23), the valve opening regulator (24) and the eluate outlet region (25) are highlighted. This valve is used to fit the horizontal vacuum line.
  • Figure 8 is a front view of the adapted open-close valve.
  • the cartridge nozzle engaging regions (23), the valve opening regulator (24) and the eluate outlet (26) adapted by inserting a metal part at the lower end.
  • This adaptation piece can be metallic, plastic or even an extension of the valve itself.
  • the fitting may also contain metal or plastic gloves or cuffs for added mechanical strength.
  • This valve is used to fit peristaltic pump tubing through fittings (26). Adapted valves are used for coupling the cartridges during the conditioning, sample application, flushing and elution steps when control is performed by the peristaltic pump.
  • the present utility patent application further comprises the use of the system described for any solid phase extraction process, whether or not coupled to a vacuum pump and / or a peristaltic pump.

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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)

Abstract

La présente demande de modèle d'utilité concerne un dispositif de type "collecteur" pour extraction en phase solide, permettant l'extraction simultanée et individualisée de plusieurs cartouches et disques d'extraction. Cet équipement présente un ensemble de valves qui sont raccordées à une ligne de vide et commandées par celle-ci et un autre ensemble de valves qui sont raccordées à une pompe péristaltique et commandées par celle-ci.
PCT/BR2011/000463 2011-09-30 2011-12-07 Dispositif pour l'extraction en phase solide de type "collecteur" avec chambre à vide, valves pour commande par vide et valves adaptées pour commande par pompe péristaltique WO2013044331A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
BRMU9101903U BRMU9101903Y1 (pt) 2011-09-30 2011-09-30 dispositivo para extração em fase sólida tipo "manifold" com câmara de vácuo, válvulas para controle por vácuo e válvulas adaptadas para controle por bomba peristáltica
BRMU9101903 2011-09-30

Publications (1)

Publication Number Publication Date
WO2013044331A1 true WO2013044331A1 (fr) 2013-04-04

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PCT/BR2011/000463 WO2013044331A1 (fr) 2011-09-30 2011-12-07 Dispositif pour l'extraction en phase solide de type "collecteur" avec chambre à vide, valves pour commande par vide et valves adaptées pour commande par pompe péristaltique

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BR (1) BRMU9101903Y1 (fr)
WO (1) WO2013044331A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9802480B2 (en) 2014-11-14 2017-10-31 Toyota Jidosha Kabushiki Kaisha High-pressure tank

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2427467A (en) * 2004-11-13 2006-12-27 Hossein Salar Amoli Solid phase extraction apparatus
EP1948339B1 (fr) * 2005-10-13 2011-06-08 Xendo Holding B.V. Dispositif pour separations chromatographiques
BRMU8903082U2 (pt) * 2009-12-22 2011-08-23 Unicamp dispositivo com válvulas e vias para controle do sistema de extração em fase sólida manifold

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2427467A (en) * 2004-11-13 2006-12-27 Hossein Salar Amoli Solid phase extraction apparatus
EP1948339B1 (fr) * 2005-10-13 2011-06-08 Xendo Holding B.V. Dispositif pour separations chromatographiques
BRMU8903082U2 (pt) * 2009-12-22 2011-08-23 Unicamp dispositivo com válvulas e vias para controle do sistema de extração em fase sólida manifold

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9802480B2 (en) 2014-11-14 2017-10-31 Toyota Jidosha Kabushiki Kaisha High-pressure tank

Also Published As

Publication number Publication date
BRMU9101903Y1 (pt) 2018-12-04
BRMU9101903U2 (pt) 2013-08-13

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