Abstract:
A composite paramagnetic particle and method of making are provided. In one aspect of the invention, a particle comprising a multitude of submicron polymer bead aggregates covalently cross-linked to each other to form larger diameter particles is presented. Distributed throughout the composite paramagnetic particle are vacuous cavities. Each submicron polymer bead has distributed throughout its interior and surface submicron magnetite crystals. In another aspect of the invention, composite particles are made using high energy ultrasound during polymerization of one or more vinyl monomers. In one embodiment, high energy ultrasound is used during an emulsification step and during the early stages of the polymerization process to produce micron sized composite paramagnetic particles. The particles according to the invention exhibit a high percent magnetite incorporation and water and organic solvent stability.
Abstract:
A solid phase magnetic support having a hydrophilic surface, a method of making the support, and a method of using the support for peptide synthesis are provided. The solid phase magnetic support is synthesized from a starting material which is a magnetic polystyrene polymer bead which has a plurality of polystyrene coated metal oxide particles randomly distributed in a polystyrene matrix having chloromethyl groups. Hydrophilic long chain hydrocarbon spacer arms, such as polyalkylene diamine molecules are coupled with sonication to the chloromethyl groups. Each spacer arm is provided with a terminal amine for linking to a first amino acid. Preferably, the terminal amine on the spacer arm is provided by a low molecular weight linker molecule which can be acid cleaved from the spacer arm. However, the spacer arm may be derivatized and linked to a first amino acid which cannot be acid cleaved from the spacer arm. The inventive support can be used for automated peptide synthesis or as a support for a bound ligand in bioassays. The support is held in place magnetically while the surrounding solution is siphoned off allowing simultaneous separation of the support bound component from the reactants in solution and washing.
Abstract:
This invention provides a novel composite magnetic bead and a method for making the composite magnetic bead. The composite magnetic bead is comprised of a matrix formed from vinyl monomers throughout which is distributed primary beads, each primary bead of which is a magnetizable metal oxide encapsulated in a rigid polymeric coating. The matrix structure allows the composite magnetic bead to swell in organic solvents without loss of the intermeshed primary beads. Further, the matrix can be functionalized to allow the covalent bonding of sites useful for organic syntheses. The composite magnetic beads are made utilizing a core-shell polymerization techinque under conditions which preserve the oxidation state of the magnetizable metal oxide in the primary particles. In one embodiment, primary beads, each having a hydrophobic exterior surface, are dispersed in an inert solvent with a vinyl monomer and a crosslinking agent for that monomer to form a dispersed phase. The dispersed phase is mixed into an aqueous solvent-dispersing agent phase and stirred until the desired droplet size is achieved, then polymerization is initiated. After removal of the solvent and unreacted components, the composite magnetic beads are dried and sieved.
Abstract:
An apparatus for facilitating the running of multiple simultaneous solid phase reactions for mounting on a temperature controllable water bath and a method of using this apparatus in the presence or absence of paramagnetic beads to perform chemical syntheses resulting in separation and recovery of a final desired reaction product is provided. The apparatus comprises a reaction plate, a reaction vessel for mounting in the reaction plate, a reaction plate holder, a screw-like rod, a mounting block attached to the reaction plate holder for operably receiving the screw-like rod, a motor, a sonication region in the water bath and a magnetic separation region in the water bath. Paramagnetic beads having reaction sites are introduced into the reaction vessels along with the appropriate solvent and one or more reactants. The contents of the reaction vessel are sonicated, then moved to the magnetic separation region where the paramagnetic beads are tightly held against the reaction vessel while the solvent is aspirated off. Once the desired reaction product is attained, the reaction product is cleaved off the paramagnetic bead. In an alternative embodiment, chemical synthesis is performed in a similar manner in the absence of the paramagnetic beads.
Abstract:
A method for photochemical cleavage of carbon-sulfur bonds in conjunction with solid-phase synthesis utilizing a deoxygenated solvent and light to cleave the carbon-sulfur bond from a heterogeneous support. Also disclosed are compounds for use with said photochemical cleavage and methods of preparing them.