IP Library Granted Patent US 10,273,539
Granted Patent B2
US 10,273,539 · App. 15/343,279 · Granted Apr 30, 2019

Methods of using nucleotide analogues

Inventors: Mong Sano Marma (Natick, MA); Jerzy Olejnik (Brookline, MA)
Assignee: QIAGEN SCIENCES, LLC
C12Q1/6869C07C323/12C07C323/60C07D207/46C07F7/1804C07H19/10C07H19/14C09B1/00C09B5/2436C09B11/24C09B23/083C09B23/166C12Q1/6811C12Q1/6876C07C2603/18Y02P20/55
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Quick Facts
Patent No.
US 10,273,539
App. No.
15/343,279
Granted
Apr 30, 2019
Kind
B2
Abstract

The present invention provides methods, compositions, mixtures and kits utilizing deoxynucleoside triphosphates comprising a 3′-O position capped by a group comprising methylenedisulfide as a cleavable protecting group and a detectable label reversibly connected to the nucleobase of said deoxynucleoside. Such compounds provide new possibilities for future sequencing technologies, including but not limited to Sequencing by Synthesis.

Claims (41)

1. A method of performing a DNA synthesis reaction comprising the steps of

a) providing a nucleic acid template with a primer hybridized to said template, a DNA polymerase, at least one deoxynucleoside triphosphate having the structure:

 wherein D is a cleavable protecting group selected from the group consisting of an disulfide alkyl, disulfide substituted alkyl groups, disulfide allyl, and disulfide substituted allyl groups; B is a nucleobase; Linker comprises a cleavable oxymethylenedisulfide-containing site core, wherein said cleavable site core is selected from the group consisting of:

 wherein R 1 and R 2 are independently selected alkyl groups; and Label is a detectable label selected from the group consisting of fluorophore dyes, energy transfer dyes, mass-tags, biotin, and haptenes, and

b) subjecting said reaction mixture to conditions which enable a DNA polymerase catalyzed primer extension reaction.

2. The method according to claim 1 , wherein said DNA polymerase catalyzed primer extension reaction is part of a sequencing reaction.

3. A method for analyzing a DNA sequence comprising the steps of

a) providing a nucleic acid template with a primer hybridized to said template forming a primer/template hybridization complex,

b) adding DNA polymerase, and a first deoxynucleoside triphosphate having the structure:

 wherein D is a cleavable protecting group selected from the group consisting of an disulfide alkyl, disulfide substituted alkyl groups, disulfide allyl, and disulfide substituted allyl groups; B is a nucleobase; Linker comprises a cleavable oxymethylenedisulfide-containing site core, wherein said cleavable site core is selected from the group consisting of:

 wherein R 1 and R 2 are independently selected alkyl groups; and Label is a detectable label selected from the group consisting of fluorophore dyes, energy transfer dyes, mass-tags, biotin, and haptenes,

c) subjecting said reaction mixture to conditions which enable a DNA polymerase catalyzed primer extension reaction so as to create a modified primer/template hybridization complex, and

d) detecting said first detectable label of said deoxynucleoside triphosphate in said modified primer/template hybridization complex.

4. The method according to claim 3 , further comprising the steps of e) removing said cleavable protecting group, and f) repeating steps b) to e) at least once.

5. The method according to claim 4 , wherein the method further comprises adding a second deoxynucleoside triphosphate during repeat of step b), wherein said second deoxynucleoside triphosphate comprises a second detectable label attached via a cleavable oxymethylenedisulfide linker, wherein said second detectible label is different from said first detectible label.

6. The method according to claim 5 , wherein the nucleobase of said second deoxynucleoside triphosphate is different from the nucleobase of said first deoxynucleoside triphosphate.

7. The method according to claim 4 , wherein a mixture of at least 4 differently labeled, 3′-O methylenedisulfide capped deoxynucleoside triphosphate compounds representing analogs of Adenosine, Guanosine, Cytidine, and Thymidine or Uridine are used in step b).

8. The method according to claim 4 , wherein step e) is performed by exposing said modified primer/template hybridization complex to a reducing agent.

9. The method according to claim 8 , wherein said reducing agent is tris(2-carboxyethyl)phosphine.

10. The method according to claim 4 , wherein step e) is performed by exposing said modified primer/template hybridization complex to a thiol-containing compound.

11. The method according to claim 3 , wherein said detecting allows for the determination of the nucleobase of said incorporated first deoxynucleoside triphosphate.

12. The method according to claim 4 , wherein said detectable label from said modified primer/template hybridization complex is removed prior to step e).

13. A method of performing a DNA synthesis reaction comprising the steps of

a) providing a nucleic acid template with a primer hybridized to said template, a DNA polymerase, at least one deoxynucleoside triphosphate having the structure:

 wherein D is a cleavable protecting group selected from the group consisting of an disulfide alkyl, disulfide substituted alkyl groups, disulfide allyl, and disulfide substituted allyl groups; B is a nucleobase; A is an attachment group selected from the group consisting of propargyl, exocyclic amine, propargyl amine, and propargyl hydroxyl; C is a cleavable site core selected from the group consisting of:

 wherein R 1 and R 2 are independently selected alkyl groups; L 1 and L 2 are connecting groups; and Label is a detectable label selected from the group consisting of fluorophore dyes, energy transfer dyes, mass-tags, biotin, and haptenes, and

b) subjecting said reaction mixture to conditions which enable a DNA polymerase catalyzed primer extension reaction.

14. The method according to claim 13 , wherein said DNA polymerase catalyzed primer extension reaction is part of a sequencing reaction.

15. The method according to claim 13 , wherein L 1 is selected from the group consisting of —CONH(CH 2 ) x —, —CO—O(CH 2 ) x —, —CONH—(OCH 2 CH 2 O) x —, —CO—O(CH 2 CH 2 O) x —, and —CO(CH 2 ) x —, wherein x is 0-10.

16. The method according to claim 13 , wherein L 2 is selected from the group consisting of

—NH—, —(CH 2 ) x —NH—, —C(Me) 2 (CH 2 ) x NH—, —CH(Me)(CH 2 ) x NH—, —C(Me) 2 (CH 2 ) x CO—, —CH(Me)(CH 2 ) x CO—, —(CH 2 ) x OCONH(CH 2 ) y O(CH 2 ) z NH—, —(CH 2 ) x CONH(CH 2 CH 2 O) y (CH 2 ) z NH—, —(CH 2 ) x OCONH(CH 2 CH 2 O) y (CH 2 ) z NH—, —CONH(CH 2 ) x —, and —CO(CH 2 ) x —, wherein x, y, and z are each independently selected from is 0-10.

17. A method for analyzing a DNA sequence comprising the steps of

a) providing a nucleic acid template with a primer hybridized to said template forming a primer/template hybridization complex,

b) adding DNA polymerase, and a first deoxynucleoside triphosphate having the structure:

 wherein D is a cleavable protecting group selected from the group consisting of an disulfide alkyl, disulfide substituted alkyl groups, disulfide allyl, and disulfide substituted allyl groups; B is a nucleobase; A is an attachment group selected from the group consisting of propargyl, exocyclic amine, propargyl amine, and propargyl hydroxyl; C is a cleavable site core selected from the group consisting of:

 wherein R 1 and R 2 are independently selected alkyl groups; L 1 and L 2 are connecting groups; and Label is a detectable label selected from the group consisting of fluorophore dyes, energy transfer dyes, mass-tags, biotin, and haptenes,

c) subjecting said reaction mixture to conditions which enable a DNA polymerase catalyzed primer extension reaction so as to create a modified primer/template hybridization complex, and

d) detecting said first detectable label of said deoxynucleoside triphosphate in said modified primer/template hybridization complex.

18. The method according to claim 17 , wherein L 1 is selected from the group consisting of —CONH(CH 2 ) x —, —CO—O(CH 2 ) x —, —CONH—(OCH 2 CH 2 O) x —, —CO—O(CH 2 CH 2 O) x —, and —CO(CH 2 ) x —, wherein x is 0-10.

19. The method according to claim 17 , wherein L 2 is selected from the group consisting of

—NH—, —(CH 2 ) x —NH—, —C(Me) 2 (CH 2 ) x NH—, —CH(Me)(CH 2 ) x NH—, —C(Me) 2 (CH 2 ) x CO—, —CH(Me)(CH 2 ) x CO—, —(CH 2 ) x OCONH(CH 2 ) y O(CH 2 ) z NH—, —(CH 2 ) x CONH(CH 2 CH 2 O) y (CH 2 ) z NH—, —(CH 2 ) x OCONH(CH 2 CH 2 O) y (CH 2 ) z NH—, —CONH(CH 2 ) x —, and —CO(CH 2 ) x —, wherein x, y, and z are each independently selected from is 0-10.

Assignments (8)
RELEASE OF SECURITY INTEREST Recorded Mar 24, 2023
From: PERCEPTIVE CREDIT HOLDINGS III, LP
To: ISOPLEXIS CORPORATION
Reel/Frame 063235/0942 →
PATENT PURCHASE AGREEMENT Recorded Jul 30, 2021
From: QIAGEN SCIENCES, LLC
To: ISOPLEXIS CORPORATION
Reel/Frame 057043/0629 →
SECURITY AGREEMENT Recorded May 28, 2021
From: ISOPLEXIS CORPORATION
To: PERCEPTIVE CREDIT HOLDINGS III, LP
Reel/Frame 056421/0929 →
MERGER Recorded Nov 8, 2018
From: QIAGEN WALTHAM, INC.
To: QIAGEN SCIENCES, LLC
Reel/Frame 047923/0815 →
CHANGE OF NAME Recorded Aug 8, 2018
From: INTELLIGENT BIO-SYSTEMS, INC.
To: QIAGEN WALTHAM, INC.
Reel/Frame 046749/0267 →
MERGER Recorded Jul 31, 2018
From: QIAGEN WALTHAM, INC.
To: QIAGEN SCIENCES LLC
Reel/Frame 046519/0201 →
CHANGE OF NAME Recorded May 17, 2018
From: INTELLIGENT BIO-SYSTEMS, INC.
To: QIAGEN WALTHAM, INC.
Reel/Frame 047132/0861 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 11, 2018
From: MARMA, MONG SANO; OLEJNIK, JERZY; KORBOUKH, ILIA
To: INTELLIGENT BIO-SYSTEMS, INC.
Reel/Frame 045783/0131 →
Continuity (3)
Provisional Application 62327555 · Apr 26, 2016
Provisional Application 62251884 · Nov 6, 2015
Related Publication 20170137878A1 · May 18, 2017
Cited By (6)
US 12,188,086 US 12,215,122 US 12,215,124 US 12,337,009 US 12,503,730 US 12,595,508