L-lysine Salt Crystallization of Rx100 Phosphorothioate

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

The existing forms of (Z)-O-octadec-9-en-1-yl O,O-dihydrogen phosphorothioate (Rx100) have poor stability, solubility, and handling issues due to its oily nature and sensitivity, and previous attempts to form desirable salt forms like sodium or potassium salts have been unsuccessful, leading to instability and impurity incorporation.

Innovation Solution

Formation of crystalline or semi-crystalline salts with L-lysine base, specifically mono-, sesqui-, or di-L-lysine salts, which exhibit improved solubility, stability, and purity, and are characterized by XRPD, NMR, and thermal analysis, resulting in a more stable and filterable form.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If Rx100.FA is stored at less than -20°C, then short-term stability is preserved, but handling difficulty and operational complexity increase

Engineering Contradiction:
ImprovestabilityVSAvoidhandling
Core Design Contradiction:
Stability of the object's compositionVSEase of operation

Solution Approach 1:

The patent transforms the physical state parameter of Rx100 from oily liquid to crystalline solid through salt formation with L-lysine, enabling storage at ambient temperatures while maintaining stability, thus eliminating the need for cold storage and improving handling ease

Inventive Principle:
Principle #35Parameter changes

2Quantity of substance

If sodium or potassium salts are formed, then solubility may improve, but filterability deteriorates as they fail to yield filterable solids

Engineering Contradiction:
ImprovesolubilityVSAvoidfilterability
Core Design Contradiction:
Quantity of substanceVSEase of manufacture

Solution Approach 1:

The patent changes the counterion parameter from sodium/potassium to L-lysine, which enables the formation of filterable crystalline solids that maintain good solubility properties, simultaneously satisfying both filterability and solubility requirements

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If ammonia salt is formed through freeze-drying, then a solid powder is obtained, but stability and purity worsen due to ammonia loss, moisture absorption, and impurity incorporation

Engineering Contradiction:
Improvesolid formVSAvoidstability
Core Design Contradiction:
Ease of manufactureVSStability of the object's composition

Solution Approach 1:

The patent replaces the unstable ammonia salt with L-lysine salt that does not lose its counterion during storage, eliminating the need for freeze-drying and providing a stable solid form that resists moisture absorption and impurity incorporation

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent changes the counterion from ammonia to L-lysine, which provides a stable crystalline solid that maintains its composition during storage and handling, improving both stability and purity

Inventive Principle:
Principle #35Parameter changes

4Ease of operation

If Rx100.FA is used in oily form, then it is easy to handle initially, but stability and solubility deteriorate over time

Engineering Contradiction:
ImprovehandlingVSAvoidstability
Core Design Contradiction:
Ease of operationVSStability of the object's composition

Solution Approach 1:

The patent transforms the physical state from oily liquid to crystalline solid through salt formation, which improves long-term stability and solubility while maintaining ease of handling in solid form through standard pharmaceutical processing

Inventive Principle:
Principle #35Parameter changes

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

The L-lysine salts of Rx100 display enhanced stability, solubility, and reduced impurity levels, offering a more practical and effective pharmaceutical form for use, particularly in mitigating gastrointestinal acute radiation syndrome by activating LPAR2 receptors.

Implementation Method 1

Formation of crystalline or semi-crystalline salts with L-lysine base

Methodology Applied
Scientific EffectIonic bonding: Chemical Bonding

Implementation Method 2

characterized by XRPD, NMR, and thermal analysis

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Implementation Method 3

characterized by XRPD, NMR, and thermal analysis

Methodology Applied
Scientific EffectNuclear magnetic resonance: Magnetic Field

Data Source

PatentEP3089986B1Crystalline salts of (z)-o-octadec-9-en-1-yl o,o-dihydrogen phosphorothioate
Publication Date: 2019.06.26 RXBIO
  • EP3089986B1 patent drawingFigure 1
  • EP3089986B1 patent drawingFigure 2
  • EP3089986B1 patent drawingFigure 2a

AI summary

Here provided are a salt of Z)-O-octadec-9-en-1-yl O,O-dihydrogen phosphorothioate with an L-lysine addition in crystalline form and methods of making and using the same.