Polymeric solid supports for chromatography nanocolumns
First Claim
1. An in situ frit for immobilizing a stationary phase material in a chromatography nanocolumn comprising an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), wherein said particles are suspended in said network.
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Abstract
Nanocolumn chromatography devices useful, e.g., in CEC and nanoLC are disclosed. An exemplary chromatography device of the invention includes a nanocolumn, e.g., a capillary, packed with a particulate stationary phase material and a solid support. The solid support, or in situ frit, is adjacent to and integral with the stationary phase material. An in situ frit of the invention may be a mixture of the stationary phase material and a polymeric network of cross-linked poly(diorganosiloxane), e.g., poly(dimethylsiloxane), which may optionally be sintered. The invention also provides methods of making and using such devices.
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Citations
120 Claims
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1. An in situ frit for immobilizing a stationary phase material in a chromatography nanocolumn comprising an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), wherein said particles are suspended in said network.
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2. A medium for molecular separations comprising
a) a particulate stationary phase material; - and
b) an in situ frit adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network.
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3. A column chromatography device comprising
a) a nanocolumn having a cylindrical interior for accepting a stationary phase; -
b) a particulate stationary phase material packed within said nanocolumn; and c) an in situ frit within said nanocolumn, and adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network. - View Dependent Claims (5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 54, 55, 56, 57, 58, 112, 113, 114)
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4. A chromatography device prepared by the steps of providing a nanocolumn having a cylindrical interior for accepting a stationary phase, and forming a stationary phase within said nanocolumn, wherein said stationary phase comprises
a) a particulate stationary phase material; - and
b) an in situ frit adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network.
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50. A method of making a chromatography device comprising the steps of
a) providing a nanocolumn having a cylindrical interior for accepting a stationary phase; -
b) forming a stationary phase within said nanocolumn, wherein said stationary phase comprises i) a particulate stationary phase material; and ii) an in situ frit adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network; c) curing the stationary phase within said nanocolumn; and d) optionally sintering the stationary phase within said nanocolumn. - View Dependent Claims (60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99, 100, 101, 102, 103, 104, 105, 106, 107, 108, 109, 110, 111, 115, 116, 117, 120)
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51. A separations instrument comprising a (i) column chromatography device and at least one component selected from a (ii) detecting means, an (iii) introducing means, or an (iv) accepting means, wherein
(i) said column chromatography device comprises a) a nanocolumn having a cylindrical interior for accepting a stationary phase, b) a particulate stationary phase material packed within said nanocolumn, and c) an in situ frit within said nanocolumn, and adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network; -
(ii) said detecting means is operatively connected to said nanocolumn and is capable of measuring physicochemical properties; and (iii) said introducing means is operatively connected to said nanocolumn and is capable of conducting a liquid into said nanocolumn; and (iv) said accepting means is capable of holding said nanocolumn in a configuration in which the nanocolumn is operatively connected to either a detecting means or an introducing means. - View Dependent Claims (118, 119)
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52. A separations instrument comprising a column chromatography device comprising
a) a nanocolumn having a cylindrical interior for accepting a stationary phase; -
b) a particulate stationary phase material packed within said nanocolumn; and c) an in situ frit within said nanocolumn, and adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network.
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53. An analytical method of separating components of a mixture comprising a step of contacting said mixture with a column chromatography device comprising
a) a nanocolumn having a cylindrical interior for accepting a stationary phase; -
b) a particulate stationary phase material packed within said nanocolumn; and c) an in situ frit within said nanocolumn, and adjacent to and integral with said stationary phase material, wherein said in situ frit comprises an intimate mixture of particles comprising a stationary phase material and a polymeric network comprising cross-linked poly(diorganosiloxane), and wherein said particles are suspended in said network.
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59. A method of making a chromatography device comprising the steps of
a) preparing a mixture of a stationary phase material, a solvent, and polymer reagents that produce cross-linked poly(diorganosiloxane); -
b) introducing said mixture prepared in step (a) into an end of said nanocolumn; c) allowing the solvent to evaporate at room temperature; d) curing the dried mixture by heating the nanocolumn and the mixture therein to a temperature of between about 70°
C. to about 150°
C. for a period of time ranging from about 0.5 hours to about 3 hours to thereby produce an in situ frit; ande) optionally sintering the in situ frit by heating the nanocolumn and the in situ frit therein to a temperature of between about 250°
C. and about 350°
C. for a period of time ranging from about 5 seconds to about 30 second.
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Specification