Simultaneous Thiolation Conjugation Method

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Solution Overview

Problem

Conventional methods for producing conjugates require a separation step to remove excess thiol generator and by-products, leading to material loss and inefficiency, especially when working with small quantities of biomolecules.

Innovation Solution

A method where the thiol generator is in simultaneous contact with both chemical entities during the conjugation process, eliminating the need for a separation step and allowing immediate reaction of newly formed sulfhydryl groups with the second chemical entity, using thiolactones or iminothiolactones like 2-iminothiolane to produce thiolated antibodies that can react directly with sulfhydryl-reactive groups.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If a separation step is used to remove excess thiol generator and by-products, then purity of the conjugate is improved, but material loss increases and productivity decreases

Engineering Contradiction:
Improvepurity of the conjugateVSAvoidconjugation efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The patent extracts and removes the thiol generator from the reaction mixture after the conjugation reaction is complete, rather than requiring separation during or before the reaction. This is achieved by using a thiol generator that can be selectively removed after having served its purpose of generating sulfhydryl groups for conjugation.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The thiol generator is added to the reaction mixture before the conjugation reaction occurs, allowing it to generate sulfhydryl groups in advance. The generator remains in the mixture during the reaction and is removed only after the conjugation is complete, eliminating the need for intermediate separation steps.

Inventive Principle:
Principle #10Preliminary action

2Reliability

If a separation step is introduced to remove excess reagents, then cross-reactivity is reduced, but the complexity of the process increases

Engineering Contradiction:
Improvereduction of cross-reactivityVSAvoidprocess complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The thiol generator serves multiple functions: it generates sulfhydryl groups for conjugation, remains in the mixture during the reaction without interfering, and can be removed after the reaction is complete. The system essentially cleans itself by allowing the generator to be removed after serving its purpose, rather than requiring complex separation apparatus.

Inventive Principle:
Principle #25Self-service

3Quantity of substance

If conventional thiol generation methods are used, then sulfhydryl groups are produced, but material loss occurs due to required separation steps

Engineering Contradiction:
Improveamount of biomoleculeVSAvoidmaterial loss
Core Design Contradiction:
Quantity of substanceVSLoss of substance

Solution Approach 1:

The thiol generator continues to function throughout the conjugation reaction, generating sulfhydryl groups as needed without requiring removal or interruption. The useful action of the generator (producing sulfhydryl groups) continues continuously from the start of the reaction until completion, maximizing the utilization of the biomolecule.

Inventive Principle:
Principle #20Continuity of useful action

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This approach simplifies the conjugation process, reduces material loss, enables direct labelling of proteins on any scale, enhances reproducibility, and lowers costs by allowing conjugation with small amounts of materials and reducing unwanted cross-reactivity.

Implementation Method 1

The thiol generator (TG) contains one or more sulphur atoms and reacts with the first chemical entity (A) to produce a covalently bound sulfhydryl (or thiol) group on the first chemical entity, the sulfhydryl group including a sulphur atom from the thiol generator.

Methodology Applied
Scientific EffectRing-opening reaction:

Implementation Method 2

The thiol generator (TG) contains one or more sulphur atoms and reacts with the first chemical entity (A) to produce a covalently bound sulfhydryl (or thiol) group on the first chemical entity

Methodology Applied
Scientific EffectRearrangement reaction:

Implementation Method 3

The sulfhydryl group derived from A is almost always incorporated either as a stable thioether bond or as one half of a reversible (reducible) disulphide bridge between A and B.

Methodology Applied
Scientific EffectThioether bond formation: Chemical Bonding

Implementation Method 4

The sulfhydryl group derived from A is almost always incorporated either as a stable thioether bond or as one half of a reversible (reducible) disulphide bridge between A and B.

Methodology Applied
Scientific EffectDisulphide bridge formation: Chemical Bonding

Data Source

PatentEP1968641B1Production of conjugates
Publication Date: 2014.06.11 INNOVA BIOSCI
  • EP1968641B1 patent drawingFigure 1~2
  • EP1968641B1 patent drawingFigure 3~4
  • EP1968641B1 patent drawingFigure 5~6

AI summary

A method of reacting a first chemical entity and a second chemical entity to form a conjugate in which the first and second chemical entities are covalently bound with respect to each other, comprises bringing into simultaneous contact the first chemical entity, the second chemical entity and a thiol generator, wherein the thiol generator reacts with the first chemical entity in a thiolation reaction resulting in formation of a free sulfhydryl group on the first chemical entity, and the free sulfhydryl group reacts with the second chemical entity to form the conjugate, and wherein the second chemical entity is polyvalent with respect to its reactivity with sulfhydryl groups. The present invention primarily differs from the prior art in that no separation step is involved between reaction of the thiol generator and first chemical entity and reaction with the second chemical entity. The invention also provides a conjugation kit.