Integrated instrument for supercritical fluid sample extraction, sample separation and concentration
AssigneeAnalytical Bio-Chemistry Laboratories, Inc.
InventorsDavid L. Stalling, Said Saim
Life of this patent
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Abstract
An integrated sample extraction and separation system includes a number of substantially identical supercritical fluid extraction modules and sample separation modules connected in common to a source of supercritical fluid and modifier and to instruments for sample analysis. Each of the supercritical fluid extraction columns is provided with separate pressure and temperature controls. Preferably, each sample separation module provides the choice of sample separation by dissolving the extracted sample in solvent, by adsorption, or by size exclusion chromatography. Either the supercritical fluid or various solvents may be used as the mobile phase in the sample separation step.
Claims50
An apparatus for supercritical fluid extraction of a sample from a bulk matrix, followed by supercritical fluid separation of the extracted sample into its constituents, comprising a number of separate supercritical fluid extraction modules with independent temperature, pressure, and flow rate control, said apparatus further comprising:
- supply means for supply of a supercritical fluid,
- a plurality of supercritical fluid sample extraction columns, each having an inlet and an outlet, and being constructed to contain said supercritical fluid,
- means for individually establishing fluid flow communication between the inlets of individual ones of said extraction columns and said supply means in order to extract a sample from a matrix disposed in the sample extraction column;
- and
- a like plurality of sample separation means, each having an inlet in fluid flow communication with the outlet of a corresponding respective sample extraction column, for separating the extracted sample into its constituents.
An instrument for sample analysis, comprising supercritical fluid extraction apparatus for extraction of analytical samples from sample matrices, said apparatus further comprising:
- a source of supercritical fluid;
- a source of modifier solvent;
- means for proportional mixing of said supercritical fluid with said modifier solvent;
- and
- a plurality of supercritical fluid extraction columns, each comprising a pressure vessel having an inlet in fluid communication with said means for proportional mixing, and an outlet;
- a like plurality of means for separation of a sample extracted from a sample matrix in one of said extraction columns into its constituents, each said means for separation being in fluid communication with a corresponding outlet of one of said pressure vessels;
- and
- means for separately controlling the pressure and temperature in and flow rate of fluid through each of said columns.
An apparatus for supercritical fluid extraction of a sample from a matrix followed by supercritical fluid separation of the sample into its constituent parts, comprising a number of separate supercritical fluid extraction modules with independent temperature, pressure, and flow rate control, said apparatus comprising:
- a source of supercritical fluid, a plurality of supercritical fluid sample extraction columns, and a like plurality of corresponding sample separation units, at least some of said sample separation units comprising columns packed with adsorption media or size exclusion chromatographic media, each said supercritical fluid sample extraction column having a defined inlet port normally controllably connected in flow communication with said source of supercritical fluid, and a defined outlet port normally in fluid flow communication with a corresponding sample separation unit, and further comprising piping means for controllably establishing flow communication between the source of supercritical fluid and the outlet port of each said supercritical fluid sample extraction column, whereby the supercritical fluid sample extraction column may be rinsed with said supercritical fluid.
A method of extracting a sample from a matrix, said sample containing a constituent of interest and one or more further constituents, and for subsequently separating said sample into its constituents, comprising the steps of:
- providing an instrument comprising means coacting to provide supercritical fluid extraction followed by supercritical fluid sample separation, including a number of separate supercritical fluid extraction modules with independent temperature, pressure, and flow rate control;
- placing the matrix in a supercritical fluid sample extraction column of said instrument;
- admitting supercritical fluid to the supercritical fluid sample extraction column and allowing the supercritical fluid to elute from the supercritical fluid sample extraction column together with the sample, while controlling the temperature and pressure within, and the flow rate through, said extraction column,
- admitting the eluting supercritical fluid together with the sample to a size exclusion chromatography column of said instrument, said chromatography column being packed with polystyrene divinyl benzene;
- and
- allowing the supercritical fluid to elute from said size exclusion chromatography column, such that the constituents of the sample elute from said size exclusion chromatography column together with the supercritical fluid, ordered by their relative molecular sizes.
An instrument for supercritical fluid extraction of a sample from a matrix and supercritical fluid separation of said sample into its constituents, comprising a number of separate supercritical fluid extraction modules with independent temperature, pressure, and flow rate control, and a number of sample separation modules, each of said separation modules being adapted to be placed into fluid flow communication with one of said supercritical fluid extraction modules to receive a sample eluted therefrom, and for separating said sample into its constituents, and said separation modules each further comprising:
- (1) a source of supercritical fluid;
- (2) a source of solvent;
- (3) sample separation means;
- and
- (4) controllable valve means for selectible supply of said supercritical fluid or said solvent to said sample separation means;
- said sample separation means comprising at least one of:
- (a) collection vessel means for collecting a sample eluted from the supercritical fluid sample extraction column in a quantity of solvent liquid;
- (b) absorbent means for absorbing a constituent of interest from a sample eluted from the supercritical fluid sample extraction column, and means for subsequently removing the constituent of interest from said absorbent means;
- and
- (c) size exclusion chromatography means for separating a constituent of interest from a sample eluted from the supercritical fluid sample extraction column.
Dependencies are inferred from the claim text.