WO2020215087A1

WO2020215087A1 - Chromotography analyte recovery system and method of using

Info

Publication number: WO2020215087A1
Application number: PCT/US2020/029006
Authority: WO
Inventors: Curtis EBERSOLD; Kenneth Joseph JAMES
Original assignee: Supercritical Fluid Technologies, Inc.
Priority date: 2019-04-18
Filing date: 2020-04-20
Publication date: 2020-10-22

Abstract

A chromatography analyte recovery system incorporates both sample and solvent nozzles that are configured to recover a high portion of the analyte in a collection container. The chromatography analyte recovery system utilizes a funnel configured over the collection container, whereby the sample stream, comprising the analyte, is sprayed from the sample nozzle onto the wall of the funnel and then flows down into the collection container. The collection of the sample and analyte therein is improved by the injection or spraying of a solvent stream from the solvent nozzle onto the funnel wall. In an exemplary embodiment, the solvent is injected onto the funnel wall above the sample stream, thereby producing a washing effect to wash the sample stream down into the collection nozzle. The solvents from the sample stream and from the solvent nozzle evaporate out of the collection container leaving the analyte material in the collection container.

Description

CHROMOTOGRAPHY ANALYTE RECOVERY SYSTEM AND METHOD OF USING

BACKGROUND OF THE INVENTION

Cross-Reference to Related Applications

[0001] This application claims priority to U.S. Provisional Patent Application

No. 62/835,805, filed on April 18, 2019, the disclosure of which is incorporated by reference herein in its entirety.

Field of the Invention

[0002] This application is directed to an analyte recovery system for flash chromatography systems.

Background

[0003] Chromatography systems are used to measure the chemical composition of various compounds and in some cases the compounds of interest are in short supply or are valuable compounds. Conventional chromatography systems do not effectively recovery the analyte.

SUMMARY OF THE INVENTION

[0004] The invention is directed to a chromatography analyte recovery system comprising a sample nozzle and solvent nozzle that are configured to recover a high portion of the analyte in a collection container. An exemplary chromatography analyte recovery system utilizes a funnel configured over the collection container, whereby the sample stream, comprising the analyte, is sprayed from the sample nozzle onto the wall of the funnel and then flows down into the collection container. The collection of the sample and analyte therein is improved by the injection or spraying of a solvent stream from the solvent nozzle onto the funnel wall. In an exemplary embodiment, the solvent is injected onto the funnel wall above the sample stream, thereby producing a washing effect to wash the sample stream down into the collection nozzle. The solvent from the sample stream and solvent from the solvent nozzle evaporate out of the collection container leaving the analyte material in the collection container. The solvent nozzle and sample nozzles may be configured into a nozzle assembly to facilitate proper orientation of the two steams with respect to each other and with respect to the funnel.

[0005] The solvent stream and/or sample stream may be sprayed at an offset angle to a central axis that extends up through the center of the funnel. This offset angle may be configured to ensure proper incident locations of the sample and solvent streams on the funnel wall. Again, if is preferred that the solvent stream have a solvent incident location that is above the sample incident location on the funnel wall. Likewise, the solvent stream and/or sample stream may be configured an offset distance from the central axis, again to create proper relative incident locations of the sample and solvent streams. The solvent stream and/or sample stream may be configured to be dispensed from the respective nozzles at offset distances from the central axis and may also be configured to dispense at an offset angle to the central axis.

[0006] In an exemplary embodiment, a solvent nozzle is configured to dispense a solvent stream into the collection funnel, wherein the solvent nozzle has a discharge axis that is at an offset angle to the central axis of the collection funnel to cause the solvent stream to hit the funnel wall. The offset angle of the discharge axis may be about 10 degrees or more, about 20 degrees or more, about 30 degrees or more, about 45 degrees or more, and any range between and including the offset angles provided. The solvent stream being dispensed at an offset angle may promote swirling of the solvent around the inside surface of the funnel wall to more effectively wash sampler material into the collection container. Again, the solvent stream is configured to hit the funnel wall at a solvent incident location that is higher up the funnel wall than a sample incident location. This offset in incident locations enables the solvent from the solvent stream to effectively wash the sample down through the funnel and into the collection container. The two streams, sample and solvent, may be dispensed at the same time and the solvent stream may be dispensed after the sample stream has ceased to wash the sample into the collection container. In an exemplary embodiment, the solvent stream is initiated after the sample stream has concluded to provide a final wash of the sample material down into the collection container. [0007] The chromatography analyte recovery system may be used with any type of chromatography including, but not limited to, column chromatography, gas

chromatography and flash chromatography.

[0008] The summary of the invention is provided as a general introduction to some of the embodiments of the invention, and is not intended to be limiting. Additional example embodiments including variations and alternative configurations of the invention are provided herein.

BRIEF DESCRIPTION OF SEVERAL VIEWS OF THE DRAWINGS

[0009] The accompanying drawings are included to provide a further

understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention, and together with the description serve to explain the principles of the invention.

[0010] FIG. 1 shows an exemplary analyte recovery system comprising a plurality of nozzle assemblies comprising a sample nozzle and a solvent nozzle configured over a collection funnel.

[0011] FIG. 2 shows a cross sectional view of a nozzle assembly configured over a collection funnel.

[0012] Corresponding reference characters indicate corresponding parts

throughout the several views of the figures. The figures represent an illustration of some of the embodiments of the present invention and are not to be construed as limiting the scope of the invention in any manner. Further, the figures are not

necessarily to scale, some features may be exaggerated to show details of particular components. Therefore, specific structural and functional details disclosed herein are not to be interpreted as limiting, but merely as a representative basis for teaching one skilled in the art to variously employ the present invention. DETAILED DESCRIPTION OF THE ILLUSTRATED EMBODIMENTS

[0013] As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having" or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Also, use of "a" or "an" are employed to describe elements and components described herein. This is done merely for convenience and to give a general sense of the scope of the invention. This description should be read to include one or at least one and the singular also includes the plural unless it is obvious that it is meant otherwise.

[0014] Certain exemplary embodiments of the present invention are described herein and are illustrated in the accompanying figures. The embodiments described are only for purposes of illustrating the present invention and should not be interpreted as limiting the scope of the invention. Other embodiments of the invention, and certain modifications, combinations and improvements of the described embodiments, will occur to those skilled in the art and all such alternate embodiments, combinations, modifications, improvements are within the scope of the present invention.

[0015] As shown in FIG. 1 , an exemplary analyte recovery system 10 comprises a plurality of nozzle assemblies 12, each comprising a sample nozzle 20 and a solvent nozzle 40 configured over a collection funnel 60. The sample input 32 extends from a chromatography system to provide sample comprising analyte for collection. A solvent input 34, which may comprise the same solvent used in the chromatography system extends to the nozzle assembly and is coupled with the solvent nozzle 40. The sample nozzle may dispense a sample from a chromatography system such as a flash chromatography system and may contain analyte and solvent. The sample may be dispensed into the funnel and flow down the surface of the funnel wall to the collection container 70. The sample nozzle discharge axis may be offset from the center of the funnel such that the sample is dispensed onto the funnel wall 62. The solvent may evaporate off as the sample flows down the funnel, thereby leaving analyte in the collection container. The solvent nozzle dispenses a solvent onto the funnel to wash any additional sample down into the collection container. The solvent nozzle may be configured with a discharge axis to dispense the solvent onto the funnel wall and preferable above the location where the sample hits the funnel wall when dispensed.

[0016] As shown in FIG. 2, an exemplary nozzle assembly 12 is configured over a collection funnel 60 and configured to dispense both a sample stream 22 and a solvent stream 42 into said funnel. The sample stream may comprise an analyte 28 and solvent 48’ and the discharge axis 24 of the sample nozzle 20 may be offset an offset distance 25 from the center axis 66 of the funnel, thereby causing the sample stream to hit the funnel wall 62. The sample then flows down the funnel wall and into the collection container 70. The solvent may evaporate off leaving only the recovered analyte 80 in the collection container and on the wall of the funnel. The solvent nozzle 40 of the nozzle assembly 12 may be configured to produce a solvent stream 42, comprising solvent 48, having an solvent axis 46 that is at an offset angle 45 from vertical, or the central axis 66, to cause the solvent stream to hit the funnel wall 62 and swirl around the funnel as it flows down into the collection container. The solvent stream may hit the funnel wall as a solvent incident location 49 that is above the sample incident location 29, where the sample stream hits the funnel wall, thereby ensuring that sample retained on the funnel wall is washed down into the collection container. Note that the solvent stream is also configured an offset distance from the central axis.

[0017] It will be apparent to those skilled in the art that various modifications, combinations and variations can be made in the present invention without departing from the scope of the invention. Specific embodiments, features and elements described herein may be modified, and/or combined in any suitable manner. Thus, it is intended that the present invention cover the modifications, combinations and variations of this invention provided they come within the scope of the appended claims and their equivalents.

Claims

What is claimed is:

1. An analyte recovery system utilizing supercritical fluid in flash chromatography

comprising:

a) a collection funnel having a funnel wall around a central axis;

b) a sample nozzle configured to dispense a sample stream comprising a

sample into the collection funnel and onto the funnel wall at a sample incident location;

c) a solvent nozzle configured to dispense a solvent stream of supercritical fluid combined with a co-solvent, the stream maintained at a continuous pressure of between about 500 psi and about 10,000 psi, into the collection funnel and onto the funnel wall at a solvent incident location that is above the sample incident location;

wherein the sample stream is dispensed into the collection funnel and wherein the sample flows down the collection funnel into a collection container; wherein the solvent stream is dispensed after the sample stream to wash said sample into the collection container.

2. The analyte recovery system of claim 1 , wherein the solvent stream is dispensed after the sample stream is completed dispensing to wash said sample into the collection container.

3. The analyte recovery system of claim 1 , wherein the solvent nozzle has a discharge axis that is at an offset angle to the central axis of the collection funnel to cause the solvent stream to hit the funnel wall.

4. The analyte recovery system of claim 3, wherein the offset angle of the discharge axis of the solvent nozzle is at least 10 degrees.

5. The analyte recovery system of claim 3, wherein the offset angle of the discharge axis of the solvent nozzle is at least 20 degrees.

6. The analyte recovery system of claim 3, wherein the sample nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel and wherein the sample stream hits the funnel wall.

7. The analyte recovery system of claim 1 , wherein the sample nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel and wherein the sample stream hits the funnel wall.

8. The analyte recovery system of claim 7, wherein the solvent nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel to cause the solvent stream to hit the funnel wall.

9. The analyte recovery system of claim 1 , wherein the sample nozzle has a discharge axis that is at an offset angle to the central axis of the collection funnel to cause the solvent stream to hit the funnel wall, and wherein the solvent nozzle has a discharge axis that is at an offset angle to the central axis of the collection funnel to cause the solvent stream to hit the funnel wall.

10. The analyte recovery system of claim 9, wherein the sample nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel and wherein the sample stream hits the funnel wall; and wherein the solvent nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel and wherein the solvent stream hits the funnel wall.

11. The analyte recovery system of claim 1 , wherein the sample nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel and wherein the sample stream hits the funnel wall; and wherein the solvent nozzle has a discharge axis that is offset an offset distance from the central axis of the collection funnel and wherein the solvent stream hits the funnel wall.

12. The analyte recovery system of claim 1 , wherein the solvent stream is decompressed at least 1500 psi down to atmospheric pressure to collect the sample through the nozzle assembly with 95% plus efficiency.