Glucuronoxylan Sulfate Preparation via Double Sulfation

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Solution Overview

Problem

Current methods for producing pentosan polysulfate (PPS) face challenges in achieving consistent high sulfation levels and molecular weight ranges, leading to variable clinical outcomes due to inconsistencies in the degree and position of sulfate groups along the glycan chain, which affects its therapeutic efficacy.

Innovation Solution

The development of glucuronoxylan sulfate (GXS) with a specific configuration of sulfate groups and a novel double sulfation method using pyridine chlorosulfonic acid complex in DMF, followed by ultrafiltration and selective fractionation with an organic solvent to achieve high and full sulfation, resulting in a consistent molecular weight range and improved therapeutic efficacy.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional sulfation methods are used to produce pentosan polysulfate, then production is simpler and faster, but the degree of sulfation is inconsistent and clinical outcomes are variable

Engineering Contradiction:
Improvedegree of sulfation consistencyVSAvoidsulfation process complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The sulfation process is divided into multiple sequential stages with controlled reaction times and conditions. Each stage targets specific hydroxyl groups on the pentosan chain, enabling progressive and consistent sulfation. This segmentation allows precise control over the degree of sulfation while maintaining reproducible clinical outcomes.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The invention systematically varies critical process parameters including temperature, reaction time, solvent composition, and reagent concentration across different sulfation stages. By optimizing and controlling these parameters, the process achieves consistent high-degree sulfation (>18%) while managing process complexity through defined parameter ranges.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If PPS with high variation in degree of sulfation is used, then production is easier and less costly, but clinical efficacy varies significantly

Engineering Contradiction:
Improveclinical efficacy consistencyVSAvoidmanufacturing simplicity
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The process incorporates analytical monitoring (NMR, capillary zone electrophoresis) at intermediate and final stages to measure the degree of sulfation. This feedback allows real-time adjustment of reaction conditions to maintain consistent sulfation levels, ensuring reliable clinical efficacy while managing manufacturing complexity through controlled monitoring points.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The invention performs preliminary optimization of sulfation conditions using model systems and small-scale experiments before full production. This preliminary action establishes standardized protocols that simplify subsequent manufacturing while ensuring consistent high-degree sulfation and reliable clinical outcomes.

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If molecular weight range is broad in PPS formulations, then more starting material is utilized, but therapeutic predictability decreases

Engineering Contradiction:
Improvemolecular weight consistencyVSAvoidmaterial utilization efficiency
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The starting pentosan material is fractionated into narrower molecular weight ranges before sulfation. This preliminary segmentation ensures that the sulfation reaction occurs on substrates of similar size, leading to more consistent molecular weight in the final product while maintaining efficient material utilization through targeted processing of defined fractions.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The invention controls molecular weight consistency by adjusting hydrolysis conditions (acid concentration, temperature, time) to produce uniform oligosaccharide chains before sulfation. This parameter control achieves narrow molecular weight distribution with improved therapeutic predictability while maintaining good material utilization.

Inventive Principle:
Principle #35Parameter changes

Data Source

PatentEP2303930B1A sulfated polysaccharide compound and the preparation and use thereof
Publication Date: 2016.02.17 PARNELL TECH
  • EP2303930B1 patent drawingFigure 1
  • EP2303930B1 patent drawingFigure 2
  • EP2303930B1 patent drawingFigure 3

AI summary

The present invention relates to a sulfated polysaccharide compound and the preparation and use thereof, and in particular to a narrow distribution low molecular weight, highly sulfated pentosan (in this instance a xylan) referred to as glucuronoxylan sulfate (GXS). The invention has been developed primarily for use in the treatment of various clinical conditions. However, it will be appreciated that the invention is not restricted this particular field of use.