Cefadroxil Crystallization pH Control for Particle Size and Color Stability

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Solution Overview

Problem

Existing crystallization processes for cefadroxil result in agglomerates with large particle size distribution and low color stability, characterized by high CIE b values.

Innovation Solution

A two-step process involving an aqueous solution of cefadroxil at a pH of 7 to 9, followed by lowering the pH to 5 to 6.5, using suitable titrants like formic acid, to achieve cefadroxil crystals with small particle size distribution and high color stability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If traditional crystallization processes are used for cefadroxil, then crystallization can be achieved, but the result is agglomerates with large particle size distribution and low color stability

Engineering Contradiction:
Improveparticle size distributionVSAvoidcolor stability
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent applies parameter changes by controlling the pH of the aqueous solution to be between 7 and 9 during crystallization, and then lowering it to between 5 and 6.5. This specific pH control mechanism transforms the crystallization process to produce crystals with small particle size distribution (10-150 μm) and high color stability (CIE b value below 6), directly resolving the contradiction between manufacturing precision and product reliability.

Inventive Principle:
Principle #35Parameter changes

2Ease of operation

If pH is not controlled during crystallization, then the process is simpler, but cefadroxil crystal explosion occurs resulting in large particle size and poor color stability

Engineering Contradiction:
Improveprocess simplicityVSAvoidparticle size distribution
Core Design Contradiction:
Ease of operationVSManufacturing precision

Solution Approach 1:

The patent introduces pH control as a critical parameter change to prevent crystal explosion during crystallization. By maintaining pH between 7 and 9 and then lowering to 5-6.5, the process achieves both operational feasibility and manufacturing precision, producing crystals with particle size distribution of 10-150 μm without excessive complexity.

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 process yields cefadroxil crystals with particle sizes between 10 to 150 μm and low CIE b values, maintaining stability for extended storage periods, significantly improving color stability and particle size distribution compared to traditional methods.

Implementation Method 1

a process for the crystallisation of a β-lactam compound, such as cefadroxil

Methodology Applied
Scientific EffectCrystallisation: Crystallisation

Implementation Method 2

bringing an aqueous solution of cefadroxil at a pH of between 7 to 9 with a suitable titrant; and lowering the pH to a value of between 5 and 6.5

Methodology Applied
Scientific EffectpH adjustment through titration:

Data Source

PatentEP2754663B1Process for the crystallisation of cefadroxil monohydrate
Publication Date: 2016.10.12 DSM SINOCHEM PHARMA NETHERLANDS

AI summary

The present invention relates to a process for the preparation of cefadroxil in crystal form, comprising: a) adding an aqueous solution of cefadroxil to a crystallisation vessel and a titrant to keep a pH in the crystallisation vessel of between 7 to 9; and b) lowering the pH in the crystallisation vessel to a value of between 5 and 6.5 to obtain a suspension of the β-lactam compound in crystal form.