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US5670054A Expired / Lapsed US ⏱️ 0.0 years remaining

Method and system for identification, purification, and quantitation of reaction components

Assignee: Warner Lambert Co LLC
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Filing: 1996-04-04
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Granted: 1997-09-23
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Expires: 2016-04-04
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Abstract

Abstract An automated HPLC system separates, identifies, purifies, and quantitates complex mixtures of reaction products or natural products on a semi-preparative or preparative scale, thus enabling rapid compilation of combinatorial libraries with minimal operator involvement.

Inventors

  • 👤 Christopher Edmund Kibbey
  • 👤 Gregory Alan Robertson

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 03:23
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/80; G01N30/82; B; B01; B01J; B01J19/00; B01J19/0046; B01J2219/00; B01J2219/00274; B01J2219/0068; B01J2219/00686; B01J2219/00689; B01J2219/00702; B01J2219/00707

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 354 words
An automated method for the separation and purification of one or more compound(s) of interest from a mixture containing a plurality of components including said compound(s), comprising: a) subjecting a first sample of said mixture to separation by high performance liquid chromatography forming a stream of eluate, differing portions of said stream of eluate containing said compound(s) separated from other portions of eluate not containing said compound(s), a concentration of each of said differing portions of eluate representable by a chromatogram having a plurality of peaks extending above a baseline, each of said peaks corresponding to at least one component of said mixture, said peaks individually assigned an identifier corresponding to the position of a peak relative to other peaks; b) identifying which of said plurality of peaks correspond to compound(s) of interest; c) storing said chromatogram in digital format; d) selecting one or more peaks corresponding to compound(s) of interest for purification; e) providing a semi-preparative or preparative HPLC system having an HPLC column, said semi-preparative or preparative HPLC system employing an HPLC compatible detector having an electrical output, said electrical output applied to an analog/digital converter to produce a digitized detector signal, and having a mechanically actuatable fluid switching valve capable of directing flow of eluate from said semi-preparative or preparative HPLC column from at least one waste reservoir to at least one compound reservoir; f) selecting a threshold limit for said digitized detector signal such that excursions above said threshold limit will logically correspond to one or more compound peaks of said chromatogram; g) injecting a sample into said semi-preparative or preparative HPLC system with said mechanically actuatable fluid switching valve in position such that eluate is directed to said waste reservoir; h) comparing said digitized detector output to said threshold limit and identifying said compound peak(s); i) upon sensing a desired compound peak, actuating said mechanically actuatable fluid switching valve to direct eluate into said compound reservoir to collect a compound-containing eluate, wherein said peak identifier and said threshold limit are digitally stored in a computer, said computer performing step h) and generating actuating signals as required by step i).
Claim 2
Dependent Claim 354 words
An automated method for the separation and purification of one or more compound(s) of interest from a mixture containing a plurality of components including said compound(s), comprising: a) subjecting a first sample of said mixture to separation by high performance liquid chromatography forming a stream of eluate, differing portions of said stream of eluate containing said compound(s) separated from other portions of eluate not containing said compound(s), a concentration of each of said differing portions of eluate representable by a chromatogram having a plurality of peaks extending above a baseline, each of said peaks corresponding to at least one component of said mixture, said peaks individually assigned an identifier corresponding to the position of a peak relative to other peaks; b) identifying which of said plurality of peaks correspond to compound(s) of interest; c) storing said chromatogram in digital format; d) selecting one or more peaks corresponding to compound(s) of interest for purification; e) providing a semi-preparative or preparative HPLC system having an HPLC column, said semi-preparative or preparative HPLC system employing an HPLC compatible detector having an electrical output, said electrical output applied to an analog/digital converter to produce a digitized detector signal, and having a mechanically actuatable fluid switching valve capable of directing flow of eluate from said semi-preparative or preparative HPLC column from at least one waste reservoir to at least one compound reservoir; f) selecting a threshold limit for said digitized detector signal such that excursions above said threshold limit will logically correspond to one or more compound peaks of said chromatogram; g) injecting a sample into said semi-preparative or preparative HPLC system with said mechanically actuatable fluid switching valve in position such that eluate is directed to said waste reservoir; h) comparing said digitized detector output to said threshold limit and identifying said compound peak(s); i) upon sensing a desired compound peak, actuating said mechanically actuatable fluid switching valve to direct eluate into said compound reservoir to collect a compound-containing eluate, wherein said peak identifier and said threshold limit are digitally stored in a computer, said computer performing step h) and generating actuating signals as required by step i).
Claim 3
Dependent Claim 27 words
The method of claim 1 wherein following said step i), j) said mechanically actuatable fluid switching valve is actuated to direct said eluate to said waste reservoir.
Claim 4
Dependent Claim 23 words
The process of claim 2 wherein a plurality of compounds of interest are to be purified, further comprising repeating steps h) through j).
Claim 5
Dependent Claim 37 words
The process of claim 2 wherein said separation and purification is to be effected an n plurality of times on successive samples from the same set of heterogeneous or homogeneous mixtures, comprising repeating steps g) through j).
Claim 6
Dependent Claim 11 words
The method of claim 2 further comprising quantitating said compound-containing eluate.
Claim 7
Dependent Claim 20 words
The method of claim 5 wherein said quantitating is performed on said compound-containing eluate using HPLC employing an ELSD detector.
Claim 8
Dependent Claim 24 words
The method of claim 6 wherein said HPLC-compatible detector monitors the eluate of said preparative HPLC column as the eluate elutes from said column.
Claim 9
Dependent Claim 41 words
The method of claim 2 wherein following a conclusion of collecting a compound-containing eluate, a line providing for eluate flow between said mechanically actuatable fluid switching valve and said compound reservoir is flushed to substantially eliminate said compound from said line.
Claim 10
Dependent Claim 15 words
The method of claim 2 wherein said steps a) and b) are performed by HPLC/MS.
Claim 11
Dependent Claim 32 words
The process of claim 1 wherein said separation and purification is to be effected an n plurality of times on successive samples from the same mixture, comprising repeating steps g) through i).
Claim 12
Dependent Claim 11 words
The method of claim 1 further comprising quantitating said compound-containing eluate.
Claim 13
Dependent Claim 21 words
The method of claim 11 wherein said quantitating is performed on said compound-containing eluate using HPLC employing an HPLC compatible detector.
Claim 14
Dependent Claim 26 words
The method of claim 12 wherein said HPLC-compatible detector monitors the eluate of said semi-preparative or preparative HPLC column as the eluate elutes from said column.
Claim 15
Dependent Claim 41 words
The method of claim 1 wherein following a conclusion of collecting a compound-containing eluate, a line providing for eluate flow between said mechanically actuatable fluid switching valve and said compound reservoir is flushed to substantially eliminate said compound from said line.
Claim 16
Dependent Claim 15 words
The method of claim 1 wherein said steps a) and b) are performed by HPLC/MS.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 2000-09-22 2001-03-24 2001-09-23 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2004-09-22 2005-03-24 2005-09-23 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2008-09-22 2009-03-24 2009-09-23 $7700.00 Window Closed / Lapsed

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