WO2002018031A2 - Dispositif et methode permettant de retirer une substance particulaire en suspension - Google Patents

Dispositif et methode permettant de retirer une substance particulaire en suspension Download PDF

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Publication number
WO2002018031A2
WO2002018031A2 PCT/US2001/025571 US0125571W WO0218031A2 WO 2002018031 A2 WO2002018031 A2 WO 2002018031A2 US 0125571 W US0125571 W US 0125571W WO 0218031 A2 WO0218031 A2 WO 0218031A2
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WO
WIPO (PCT)
Prior art keywords
adapter
filtering element
filtering
mesh
suspension
Prior art date
Application number
PCT/US2001/025571
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English (en)
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WO2002018031A3 (fr
Inventor
Dariusz Wodka
Robert G. Gentles
Original Assignee
Abbott Laboratories
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 Abbott Laboratories filed Critical Abbott Laboratories
Publication of WO2002018031A2 publication Critical patent/WO2002018031A2/fr
Publication of WO2002018031A3 publication Critical patent/WO2002018031A3/fr

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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
    • B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
    • B01L3/5025—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures for parallel transport of multiple samples
    • B01L3/50255—Multi-well filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
    • B01D35/30—Filter housing constructions
    • B01D35/306—Filter mounting adapter
    • 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

  • This invention relates to a device and a method for removing particulate materials from suspensions containing chemical and/or biological materials, and, more particularly, a device and a method for isolating components of interest from such suspensions.
  • filtration devices include those in which the filter constitutes an integral part of the vessel that contains the suspension. Although these devices eliminate the need to transfer the suspension, these systems encounter limitations in terms of flexibility in application and cost. In use, these devices involve complex assembly and disassembly of components prior to filtration. Furthermore, these devices cannot be easily incorporated onto a non-dedicated automation platform. Moreover, these devices typically cannot be employed in an unattended automated process. Examples of these systems include the Argonaut QuestTM 205 synthesizer, the Argonaut QuestTM 210 synthesizer, the Robbins FlexChemTM reaction block, described in U. S. Patent No.
  • Another major class of laboratory filters is a straw-type device comprising a glass straw capped by a porous glass filter. These filters typically operate by applying a pressure differential between the interior portion and the exterior portion of the device. The resultant pressure imbalance forces the liquid component of the suspension through the porous filter into the straw, from where it can be aspirated or collected.
  • filters are relatively expensive, and they can only be employed in an automated format as part of a highly integrated system. Typical examples of these systems include the Chemspeed ASW2000 synthesizer, the PE Biosystems SolarisTM 530 synthesizer, the Argonaut NautilusTM synthesizer, and the Argonaut TridentTM synthesizer.
  • this invention provides a filtering device.
  • the device comprises a filtering element that can be attached to an adapter.
  • the filtering element comprises a mesh surrounding a cavity.
  • the mesh of the filtering element is constructed to have sufficient porosity so that hydrostatic pressure forces the liquid components of a suspension into the cavity of the filtering element from where they can be aspirated and collected.
  • at least one semi-rigid rib supports the mesh. Both the mesh and the semi-rigid rib (or ribs) are made of chemically inert material.
  • the preferred shape of the filtering element is cylindrical or frusto- conical.
  • the purpose of the adapter is to correctly position the filtering element within a vessel containing a suspension.
  • a single adapter is attached to a single filtering element.
  • a multiple adapter assembly can be used to join a plurality of adapters to a plurality of filtering elements and to position the thus-joined filtering elements in a linear or matrix format, so that a plurality of suspensions can be filtered in parallel.
  • this invention provides a method for using the filtering device in a variety of applications. These applications include, but are not limited to, sampling of suspensions, filtration of particulate materials from suspensions, and purification or isolation of chemical or biological components contained within the suspension.
  • the method for using the device requires the following steps: (a) the filtering element is attached to the adapter, (b) the filtering element is inserted into a vessel containing a suspension, and
  • the filtering element is retained within the suspension for a period of time sufficient to ensure that at least a portion of the liquid component of the suspension flows through the mesh into the cavity of the filtering element.
  • steps (a) through (c) of the above method are repeated; then, in an additional step (d), the contents of the cavity are removed, thereby effecting at least partial separation of the solid and liquid components of the suspension.
  • step (d) the liquid component of the suspension remaining in the vessel continues to flow through the mesh into the cavity of the filtering element, whereby filtration of the suspension can be completed.
  • steps (a) through (d) of the previous embodiment are repeated; upon removal of the liquid component, in an additional step (e) fresh solvent is introduced into the suspension by dispensing the solvent into the cavity of the filtering element.
  • an optional step (f) may be performed, which step involves the aspiration from the cavity of the filtering element and dispensing to the cavity of the filtering element a volume of liquid at such a rate as to substantially agitate the suspension.
  • an additional step (g) can be performed, which step involves removal of the additional solvent from the cavity of the filtering element. Steps (e), (f), and (g) can be repeated in an iterative fashion, as often as required by the particular application in which method is employed.
  • steps (a) through (g) of the method are repeated, with the exception that the solvent can be varied during each iteration, the choice of a particular solvent for a particular iteration being a function of the nature of the application.
  • the device of this invention can be applied in a number of applications.
  • the applications include, but are not limited to, sampling of suspensions, filtration of particulate material from suspensions, and purification or isolation of chemical or biological components contained within the suspension.
  • the filtering device is reusable and the same filtering element can be attached to a variety of adapters, and vice versa. Filtration can be performed on a variety of scales, from a variety of vessels, and, when required, in parallel.
  • the method can be easily integrated onto common automation platforms, as the filtering device and the method for its use do not involve complex assembly or disassembly of components.
  • the methods described herein have the advantage of specifying procedures that provide for either sampling or filtering of suspensions.
  • the methods allow the selective separation of dissolved materials by means of appropriate combinations of solvents.
  • FIG. 1 A is a perspective view illustrating one embodiment of a filtering element suitable for the filtering device of this invention.
  • FIG. 1 B is a side view in elevation of the filtering element of FIG. 1A.
  • FIG. 1 C is a top plan view of the filtering element of FIG. 1A.
  • FIG. 1 D is a side view in elevation of the filtering element of FIG. 1 A.
  • FIG. 1 E is a side view in elevation of the filtering element of FIG. 1A.
  • FIG. 1 E is identical to FIG. 1 D, with the exception that the filtering element is rotated 90° about its longitudinal axis.
  • FIG. 2A is a perspective view illustrating one embodiment of an adapter suitable for the filtering device of this invention.
  • FIG. 2B is a side view in elevation illustrating an adapter suitable for the filtering device of this invention.
  • FIG. 2C is a cross-sectional view in elevation of the adapter of FIG. 2B.
  • FIG. 2D is a bottom plan view of the adapter of FIG. 2B.
  • FIG. 2E is a cross-sectional view, greatly enlarged, of the portion of FIG. 2B bounded by line 2E-2E.
  • FIG. 2F is a side view in elevation, greatly enlarged, of the portion of FIG. 2B bounded by line 2F-2F.
  • FIG. 3A is a schematic view of a filtering element of this invention in combination with an adapter. This view illustrates the proper location of the device within a vial.
  • FIG. 3B is a schematic view of a filtering element of this invention in combination with an adapter. This view illustrates the proper location of the device within a round-bottom flask.
  • FIG. 4 is a schematic view of an array-type adapter connected to a plurality of filtering elements. This view illustrates the proper location of the device within a plurality of vials.
  • FIGS. 5A, 5B, 5C, 5D, 5E, and 5F are schematic views illustrating a method for using the filtering device of this invention.
  • FIG. 6 is a graph illustrating the kinetics of sequestration of a secondary amine from a mixture containing the secondary amine and a tertiary amine. This graph illustrates the results of Example 3.
  • the term "suspension” means a relatively coarse, noncolloidal dispersion of solid particles in a liquid.
  • Suspensions include, but are not limited to, slurries.
  • solvent means a liquid capable of dissolving another substance.
  • solvent includes, but is not limited to, organic solvents, aqueous solvents, and buffers.
  • sampling means the act or process of selecting, testing, or examining a sample, i. e., a part representative of a whole.
  • this invention provides a filtering device 10 comprising a filtering element 12 that can be attached to an adapter 14.
  • the filtering element 12 preferably has a substantially cylindrical, a substantially conical, or a substantially frusto-conical shape.
  • the material of the filtering element 12 is a mesh 16 comprising a chemically inert material. It is preferred that that material from which the mesh 16 is formed be chemically inert so that it does not interact with the components of the suspension.
  • the material from which the mesh is formed is preferably a polymeric material, such as, for example, polypropylene, polytetrafluoroethylene (e.
  • the mesh 16 surrounds a cavity 18. If the filtering element is substantially cylindrical or substantially frusto-conical in shape, one end 20 of the filtering element 12 is also preferably constructed of a mesh comprising a chemically inert material.
  • the open spaces of the mesh preferably have at least one major dimension (e. g., length, diameter) ranging from about 20 micrometers to about 150 micrometers, preferably from about 30 micrometers to about 150 micrometers, more preferably from about 50 micrometers to about 150 micrometers. This dimension is selected to ensure that the particulate material of the suspension will be excluded from the cavity 18 of the filtering element 12.
  • the mesh 16 must also have sufficient porosity to allow the liquid components of the suspension to flow into the cavity 18 of the filtering element 12 under the force of the hydrostatic pressure that is created when the filtering device 10 is used.
  • the shape of the filtering element 12 is preferably maintained by at least one rib 22, which supports the mesh 16.
  • the at least one rib 22 comprises a semi-rigid, chemically inert material.
  • the material from which the ribs 22 are formed is preferably a polymeric material, such as, for example, polypropylene.
  • the mesh 16 is preferably attached to the at least one semi-rigid rib 22 by means of thermal bonding, ultrasonic welding, or molding.
  • Another end 24 of the filtering element 12, distal from the end 20, is capable of being attached to the adapter 14.
  • the end 24 of the filtering element 12 has an orifice 25 into which an end of the adapter 14 can be inserted.
  • the end 20 of the filtering element may have sufficient area to cause the filtering element 12 to have a base at the end 20.
  • the filtering element 12 has such a base, it is preferred that at least one protrusion 26, and preferably a plurality of protrusions 26, projects from the periphery of the end 20.
  • This protrusion 26 or protrusions 26 serves to prevent the end 20 from resting on the bottom of the vessel in which the filtering element 12 is used. This separation of the end 20 from the bottom of the vessel increases the efficiency of an optional agitation step of the method of this invention, which will be discussed below.
  • the adapter 14 is preferably constructed from a chemically inert material, such as, for example, a polymeric material, such as, for example, polypropylene.
  • the filtering element 12 is preferably attached to the adapter 14 by releasable retaining means 27, as shown in FIG. 2E.
  • the adapter 14 has a substantially frusto-conical body having a first end 28 and a second end 30.
  • the shape of the adapter 14 need not be frusto-conical.
  • the adapter 14 can be cylindrical in shape.
  • the first end 28 of the adapter 14 communicates with the end 24 of the filtering element 12.
  • the second end 30 of the adapter 14 comprises a flange 32.
  • the adapter 14 comprises a wall 33 that surrounds a cavity 34.
  • the first end 28 of the adapter 14 has an orifice 36 and the second end 30 of the adapter 14 has an orifice 38 positioned in the flange 32.
  • the portion of the adapter 14 surrounding the orifice 38 is preferably beveled to aid in guiding any aspirating apparatus within the adapter 14 of the filtering device 10.
  • the slope resulting from the beveling serves as a mechanical guide to aid in properly locating any aspirating apparatus within the adapter 14.
  • the adapter 14 has two primary functions.
  • the first function is to correctly orient the filtering element 12 within a vessel 40 that contains the suspension, as shown in FIGS. 3A and 3B.
  • the filtering element 12 is preferably located centrally in the vessel 40 (i. e., equidistant from the wall 42 of the vessel 40), and the end 20 of the filtering element 12 is preferably placed near the bottom 44 of the vessel 40. Preferably, the end 20 of the filtering element 12 should not contact the bottom 44 of the vessel 40.
  • the second function is to ensure that a partial vacuum does not develop in the space between the filtering device 10 and the wall 42 of the vessel 40. These features are important for ensuring efficient use of the filtering device 10.
  • At least one rib 46 can be used to carry out the aforementioned functions.
  • the ribs 46 are sufficiently malleable to allow the facile insertion of the filtering element 12 into the vessel 40; however, the ribs 46 are still capable of accurately positioning the filtering element 12 within the opening in the neck 48 of the vessel 40.
  • the flange 32 of the adapter 14 controls the depth to which the filtering element 12 of the device 10 can be inserted into a suspension in the vessel 40.
  • FIGS. 3A and 3B illustrate how the flange 32 controls the depth to which the filtering element 12 of the device 10 is inserted in the vessel 40.
  • the filtering element 12 and the adapter 14 are separable.
  • the adapter 14 and the filtering element 12 can be of a unitary construction. This alternative, however, reduces the versatility of the filtering element 12.
  • the filtering device 10 can be used in any type of vessel 40, provided that an appropriate adapter 14 is used. Because adapters 14 can be easily manufactured and are relatively inexpensive, as compared to the filtering element 12, significant cost and flexibility advantages can be realized by offering a wide variety of adapters. While the dimensions of the adapter 14, the filtering element 12, and the vessel 40 are not critical, representative examples of dimensions will be provided in order to demonstrate the scale of these components.
  • a typical vessel suitable for use in a laboratory setting is cylindrical vessel having a length of approximately 1 3/4 inches.
  • the base of the vessel has an outside diameter of about 9/16 of an inch.
  • the top of the vessel has an outside diameter of about 7/16 of an inch.
  • the diameter of the opening of the vessel, which is at the top thereof, is about 3/8 of an inch.
  • the filtering element 12 is substantially cylindrical in shape.
  • the length of the mesh portion of the filtering element 12 is about 1 inch.
  • the outside diameter of the mesh portion of the filtering element 12 is about 7/32 of an inch.
  • the length of the portion of the filtering element 12 that connects with the adapter 14 is about 3/8 of an inch.
  • the inside diameter of this connecting portion is sufficiently large to fit over the portion of the adapter 14 that connects with the filtering element 12.
  • the diameter of the orifice 25 of the filtering element 12 is about 1/4 of an inch.
  • the adapter 14 is frusto-conical in shape.
  • One end 30 of the adapter 14 has a flange 32 that supports the filtering device 10 when that device is inserted into the vessel 40.
  • the overall length of the adapter 12 is about 7/8 of an inch.
  • the height of the flange is about 1/16 of an inch.
  • the outside diameter of the first end 28 of the adapter is about 3/16 of an inch.
  • the outside diameter of the flange 32 is about 7/16 of an inch.
  • the diameter of the cavity 34 of the adapter 14 is about 3/16 of an inch at the first end 28.
  • the diameter of the cavity 34 of the adapter 14 gradually increases along its length toward the second end 30, because the adapter 14 is frusto-conical in shape. It is preferred that the thickness of the wall of the adapter 14 and the thickness of the wall of the filtering element 12 be as small as possible in order to reduce the cost of materials; at the same time the thickness of the walls of these components should be sufficiently large to ensure structural integrity.
  • FIG. 4 shows a multiple adapter assembly 52 suitable for positioning an array of filtering elements 12 into a plurality of vessels 40.
  • the multiple adapter assembly 52 comprises a positioning plate 54 and a plurality of adapters 56.
  • the positioning plate 54 comprises a sheet, preferably made of polymeric material, having a plurality of openings 58 therein into which the plurality of adapters 56 can be inserted.
  • the adapters 56 can be identical to the single adapter 14 previously described.
  • the adapters 56 of the multiple adapter assembly 52 can be designed to have a height of such a length that the adapters 56, in combination with the positioning plate 54 can control the depth to which a filtering element 12 may be inserted into a vessel 40.
  • the adapter 56 does not need to have a flange as does the adapter 14.
  • a releasable retaining means suitable for such a purpose can be of a type similar to that of the releasable retaining means 27.
  • the areas of the positioning plate 54 of the multiple adapter assembly 52 immediately surrounding each opening 58 of the multiple adapter assembly 52 can be beveled to facilitate the insertion of liquid handling apparatus, such as tips of pipettes, into the filtering devices that are formed by the combination of the adapters 56 of the multiple adapter assembly 52 and the filtering elements 12.
  • the slope resulting from the beveling serves as a mechanical guide to aid in properly locating any aspirating apparatus into the adapters 56 of the multiple adapter assembly 52.
  • the adapters 56 of the multiple adapter assembly 52 and the positioning plate 54 of the multiple adapter assembly 52 can be of a unitary construction.
  • the adapters 56 of the multiple adapter assembly 52, the positioning plate 54 of the multiple adapter assembly 52, and the filtering elements 12 can be of a unitary construction.
  • the multiple adapter assembly 52 is capable of holding several filtering elements 12 in a linear format or a matrix format, thereby facilitating parallel filtration of a plurality of suspensions.
  • the filtering element 12 is first attached to an appropriate adapter 14. See FIGS. 3A and 3B.
  • the combination of the filtering element 12 and the adapter 14 is then inserted into a vessel 40 containing a suspension. See FIGS. 5A and 5B, where the combination of the filtering element 12 and the adapter 14 is designated by the reference numeral 10, the vessel is designated by the reference numeral 40, the suspension is designated by the letter "S” and the filtrate is designated by the letter "F”.
  • the filtering device 10 By inserting the filtering device 10 into the suspension, liquid is forced into the cavity of the filtering element by the hydrostatic pressure arising from the physical insertion of the filtering device 10 into the suspension. See FIGS. 5B and 5C.
  • the liquid can then be aspirated from the cavity of the filtering element and collected. See FIGS. 5D, 5E, and 5F.
  • the liquid component of the suspension remaining in the vessel 40 continues to flow through the mesh into the cavity of the filtering element.
  • the procedure for using a plurality of filtering elements 12 with the adapter of the type shown in FIG. 4 is substantially similar to the procedure for using the filtering element 12 with the adapter 14.
  • the main difference between the embodiments is that a plurality of filtering elements 12 and a plurality of vessels 40 are used with the adapters 56 of the type shown in FIG. 4.
  • the filtering device 10 can be employed as described above to sample a suspension of interest.
  • the filtering device 10 is inserted into a suspension, and a small volume of the filtrate is sampled and analyzed.
  • the filtering device 10 can then be removed, and the suspension subjected to the same conditions as those prior to the sampling.
  • the method allows periodic analysis of reaction mixtures occurring in suspensions. If reaction conditions permit, the filtering device 10 can be left within the suspension throughout the course of sampling.
  • an appropriate volume of fresh solvent can then be dispensed into the cavity 18 of the filtering element 12, from where it passes into the surrounding suspension as a result of the aforementioned forces. After a sufficient equilibration period, the liquid in the cavity 18 is again aspirated and collected.
  • This process is repeated a sufficient number of times to ensure that the required degree of recovery of the desired components is achieved.
  • This process can be repeated with different solvents that are selected to optimize the efficiency of the process.
  • the efficiency of the process can be improved by agitating the suspension after each addition of solvent, either by rapidly dispensing solvents through the mesh of the filtering element 12, or by a separate mechanical agitation.
  • the filtration method can be performed with solvents having gradually differing compositions.
  • the precise composition of the solvents can be modified by varying the percentage of the solvent aspirated from the suspension in each iteration of the filtration method.
  • the filtering device 10 of this invention and the method for its use are designed to be applied principally on a laboratory scale, and most commonly with suspensions comprising polystyrene beads dispersed in organic or aqueous solvents.
  • robot pipette refers to a Tecan GenesisTM robotic platform comprising with eight syringes (1 mL) equipped with standard tips employing methanol as a system fluid.
  • the vials (4 mL) used for reactions and filtrations were supplied by Kimble Glass [Art. No. 60881 A-1545].
  • the scintillation vials (20 mL) specified were supplied by the same company [Art. No. 60957-1].
  • Nuclear magnetic resonance analytical data on the product samples was acquired by means of a Varian Unity 500 MHz NMR spectrometer, and mass spectra were acquired by means of a Finnigan XSQ 7000 mass spectrometer.
  • the prototype devices used to perform the filtrations in the examples were provided by Abbott Laboratories Development Shop and were similar to those shown in FIGS. 1 , 2, 3, and 4.
  • This example demonstrates the use of this invention to filter a reaction mixture containing a reagent supported on a polymeric particle.
  • the chemical reaction associated with this reaction mixture has been described in Tetrahedron Letters, Vol. 37, No. 40. pp. 7193-7196, 1996.
  • the reaction involves a procedure for the introduction of an alkyl group onto a variety of different amines, in a process referred to as Reductive Alkylation (Scheme 1).
  • 4-Phenylbenzaldehyde [1] (0.600 g; 3.29 mmol) was dissolved in dry methanol (24 mL). Aliquots of this solution (1 mL) were distributed by means of a robotic pipette to 24 open vials (4 mL) contained in a 6 x 4 Irori block (AccuCleave®- 96 Collection Rack; Irori Product No. AC96-04-24). A different primary amine [2] was then added to each of the vials, and the resultant mixtures were agitated on a shaker for two hours.
  • a filtering device of the type shown in FIG. 4 comprising an adapter capable of accommodating a 6 x 4 array of the filtering elements was employed to insert the filtering elements into the 24 vials.
  • the filtering elements were constructed from 74 ⁇ m polypropylene mesh (Spectrum, Product No. 148495).
  • the resultant assembly was then transferred to the deck of the robotic pipette.
  • the filtration process was accomplished by the following operations executed in parallel. For each vial, the process involved the following activities:
  • Residual liquid remaining in the cavity of the filtering element was collected by means of an additional aspiration step.
  • the residual volume of approximately 0.300 mL was over-aspirated (0.600 mL) to ensure completeness of transfer.
  • Steps (14) through (20) were then repeated.
  • the resulting filtrates contained in the destination rack were then evaporated to dryness, weighed, and the crude weights determined.
  • the residues were then re- splvated in a solvent mixture (1.5 L of 1 :1 dimethyl sulfoxide/methanol) and purified by preparative HPLC (Waters Nova-Pak ® HR C18; 6 ⁇ m 6 ⁇ A; 25x100 mm; 0-95%) acetonitrile/0.1% trifluoroacetic acid over 10 min at 40 mL/min).
  • the purified products were characterized by means of Mass Spectrometric Analysis and Nuclear Magnetic Resonance Spectroscopy.
  • Example 2 The purpose of this example was to examine the efficiency of the filtration method of this invention.
  • the same type of borohydride resin as was used in Example 1 (0.065 g; 0.275 mmol) was added to three vials (4 mL) containing a solution comprising an alkyl ether of type [3] shown in Example 1 (15.6 mg, molecular weight 225.33 g/mol) in 1 mL of methanol.
  • the vials were then capped and the resulting suspensions agitated for 12 hours.
  • the vials were then uncapped, and filtering devices of the type shown in FIGS. 3A and 3B were inserted into the vials.
  • the filtering elements were constructed of a 74 ⁇ m polypropylene mesh.
  • This example demonstrates the filtration of a reaction mixture employing a sequestration agent supported on a polystyrene support. This procedure results in the removal of one of the components of the mixture and the isolation of the desired material.
  • the method for removing secondary and primary amines by means of isocyanate supported on polystyrene was described in "Polymer Reagents and Scavengers for Parallel Solution Phase Synthesis & Purification" Argonaut Technologies application Note DS-018, 1999, Rev. 3.
  • the vial was then capped and the contents were vigorously shaken by means of a shaker.
  • the cap was removed periodically, and an aliquot (10 ⁇ L) of the solution was removed from the cavity of the filtration element by means of a manual pipette.
  • the aliquot was diluted with methanol (0.5 mL) in an HPLC vial.
  • the sample thus prepared was analyzed by analytical HPLC (YMC ODS AQ; 5 ⁇ m; 4x50 mm, 0-95% MeCN/0.1% TFA over 10 min at 1.5 mL/min; retention time (R ⁇ ) for the tertiary amine [5] 3.0 min, retention time (R ⁇ ) for the secondary amine [6] 4.8 min).
  • the kinetics of sequestration of the secondary amine were monitored by measuring disappearance of the peak at 4.8 minutes. Areas under peaks of the trace produced by an evaporative light scattering (ELS) detector were integrated and the area % of the 4.8 min peak was used as a measure of the amount of the secondary amine present in the mixture. It was assumed that the concentration of the tertiary amine that could not be sequestered by the resin would be constant. The results of the measurements are shown in Table 1 , and a plot of the data is shown in FIG. 6. TABLE 1
  • the amount of the residual [6] in the mixture was calculated from the ratio of areas of resonances: 2.83 ppm of [5] (integration value 100.0) and 3.76 ppm of [6] (integration value 4.65).

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Hematology (AREA)
  • Clinical Laboratory Science (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Filtering Materials (AREA)
  • Apparatus Associated With Microorganisms And Enzymes (AREA)

Abstract

Cette invention concerne un dispositif de filtrage comprenant un élément filtrant pouvant être monté sur un adaptateur. L'élément filtrant comprend un treillis entourant une cavité. Le treillis de l'élément filtrant présente une porosité suffisante pour que les pressions hydrostatiques et mécaniques forcent les composantes liquides de la suspension dans la cavité de l'élément filtrant, d'où elles peuvent être aspirées et recueillies. Le treillis est maintenu de préférence par une nervure semi-rigide. L'invention concerne égalent une méthodes d'utilisation du dispositif filtrant dans diverses applications concernant entre autres, mais pas uniquement, l'échantillonnage de suspensions, la filtration de matériaux particulaires présents dans des suspension et la purification ou l'isolement de composants chimiques ou biologiques en suspension.
PCT/US2001/025571 2000-08-25 2001-08-15 Dispositif et methode permettant de retirer une substance particulaire en suspension WO2002018031A2 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012116932A3 (fr) * 2011-02-28 2012-11-22 Ge Healthcare Uk Limited Support d'échantillons biologiques et son procédé d'assemblage

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US9656264B2 (en) 2011-02-28 2017-05-23 Ge Healthcare Uk Limited Biological sample holder and method of assembling same

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