Microwave-assisted chromatography preparation
First Claim
1. A sample preparation apparatus for flash chromatography, comprising:
- a source of microwave radiation for applying microwave energy;
a vessel for holding reactants, solvent, products, and chromatography media;
a microwave cavity to hold said vessel, said vessel and said cavity in wave communication with said source for applying microwave energy to said reactants and said reaction solvent to accelerate the conversion of said reactants to said products;
means for adding chromatography media to said vessel to absorb said solvent and said products; and
a gas pump in gas communication with said vessel for moving gases through said vessel during the application of microwaves to the vessel to facilitate the evaporation of the solvent from the chromatography media.
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Accused Products
Abstract
An instrument and associated method are disclosed for preparing samples for column chromatography. The method includes the steps of applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products, thereafter mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography, thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy, and thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating the components of the remaining sample for identification and purification purposes.
26 Citations
77 Claims
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1. A sample preparation apparatus for flash chromatography, comprising:
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a source of microwave radiation for applying microwave energy;
a vessel for holding reactants, solvent, products, and chromatography media;
a microwave cavity to hold said vessel, said vessel and said cavity in wave communication with said source for applying microwave energy to said reactants and said reaction solvent to accelerate the conversion of said reactants to said products;
means for adding chromatography media to said vessel to absorb said solvent and said products; and
a gas pump in gas communication with said vessel for moving gases through said vessel during the application of microwaves to the vessel to facilitate the evaporation of the solvent from the chromatography media. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23)
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24. A microwave-assisted chromatography sample preparation instrument, comprising:
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a microwave source;
means for controlling the application of microwave energy from said microwave source;
a vessel in wave communication with said microwave source for evaporating solvent from a solvent-containing composition;
a gas inlet tube about said vessel for allowing make-up gas into said vessel;
a gas exit tube about said vessel for allowing solvent to evacuate said vessel; and
a gas pump in physical communication with said vessel to facilitate the evaporation of solvent;
wherein said gas pump, said gas inlet tube, and said gas exit tube create a gas flow through said vessel to evaporate solvent from the solvent-containing composition in the vessel and from the vessel during and between applications of microwave energy. - View Dependent Claims (25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37)
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38. A method of preparing samples for column chromatography, comprising:
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mixing a sample including reaction solvent with a solid phase chromatography medium;
applying microwave energy to the sample while concurrently providing a gas flow over and around the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy and the flowing gas. - View Dependent Claims (39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49)
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50. A method for microwave assisted chromatography sample preparation, comprising:
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mixing a sample dissolved in reaction solvent with a solid phase chromatography medium;
applying microwave energy to the sample to evaporate solvents therein;
creating a gas flow through a vessel to evacuate the vaporized solvents;
monitoring the temperature of the media using temperature sensors; and
moderating the temperature of the sample;
while controlling the steps of applying microwave energy, moderating the temperature of the sample, and creating a gas flow through the vessel using a microprocessor. - View Dependent Claims (51, 52, 53, 54, 55, 56)
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57. A method of preparing samples for column chromatography, comprising:
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applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products;
thereafter mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography;
thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy; and
thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating the components of the remaining sample for identification and purification purposes. - View Dependent Claims (58, 59, 60, 61, 62, 63)
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64. A method of preparing samples for column chromatography, comprising:
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applying microwave energy to a sample composition containing at least one solvent to encourage a chemical reaction and generate desired products;
mixing a scavenging composition with the sample to remove contaminants and excess reagents;
mixing an absorbent media with the sample to absorb the solvent, the media being compatible with liquid chromatography that will separate the expected products, being chemically inert to the expected products, and being added in an amount sufficient to provide a substantially dry mixture of the media and the sample, but less than an amount that overly broadens the resolution of the sample during liquid chromatography;
thereafter applying microwave energy to the dry mixture of the media and the sample to thereby encourage the solvent to evaporate under the influence of the microwave energy; and
thereafter adding the dry mixture of the media and the remaining sample to a liquid chromatography column and separating the components of the remaining sample for identification and purification purposes. - View Dependent Claims (65, 66, 67, 68, 69)
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70. A method of dry-loading samples for column chromatography, comprising:
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adding an amount of chromatography media to a vessel holding a sample, the sample being dissolved in a solvent;
evaporating the solvent using microwave energy, leaving dried chromatography media containing the sample; and
dry-loading the dried chromatography media containing the sample onto a separation chromatography column for identification and purification of the sample components. - View Dependent Claims (71, 72, 73, 74, 75, 76, 77)
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Specification