Aqueous Suspension Concentrate Formulation Stability

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Solution Overview

Problem

Formulating pyripyropene derivative I as an aqueous suspension concentrate faces challenges such as poor stability due to particle growth and agglomeration, and gelling issues, especially at high purities, which affect its use as a pesticide.

Innovation Solution

A method involving the preparation of an aqueous slurry of coarse pyripyropene derivative particles in the presence of surfactants, followed by comminution to achieve desired particle sizes, and subsequent temperature-controlled processing to stabilize the formulation without converting the compound into specific hydrate forms, thereby avoiding gelling.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If pyripyropene derivative I is formulated as an aqueous suspension concentrate using conventional methods, then the formulation can be prepared as a liquid aqueous formulation, but the formulation exhibits poor stability upon storage due to particle growth and agglomeration

Engineering Contradiction:
Improvestorage stabilityVSAvoidparticle size control
Core Design Contradiction:
Stability of the object's compositionVSReliability

Solution Approach 1:

The patent applies preliminary action by converting the pyripyropene derivative into its anhydrous form (Form B) before formulation. This pre-treatment step prevents hydrate formation during storage that would otherwise cause particle growth and agglomeration, thereby maintaining stable particle size and formulation reliability throughout storage.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent changes the physical-chemical parameter of the active ingredient by using a specific anhydrous crystalline form (Form B) with defined X-ray diffraction characteristics. This parameter change from hydrated to anhydrous form fundamentally alters the stability behavior, preventing particle growth and agglomeration during storage while maintaining reliable particle size control.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If the pyripyropene derivative I is comminuted to achieve fine particle size, then the desired particle size below 10 μm is obtained, but gelling occurs upon comminution especially at high purities

Engineering Contradiction:
Improveparticle sizeVSAvoidgelling issue
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent applies preliminary action by pre-converting the pyripyropene derivative to its anhydrous Form B before the comminution process. This pre-treatment prevents gelling during comminution by eliminating the tendency to form hydrates under the mechanical stress and moisture conditions of the comminution process, enabling successful particle size reduction to below 10 μm without manufacturing failures.

Inventive Principle:
Principle #10Preliminary action

3Stability of the object's composition

If a surfactant system is used to stabilize the suspension concentrate, then particle stability is improved, but specific hydrate forms may form that affect formulation stability

Engineering Contradiction:
Improveparticle stabilityVSAvoidhydrate formation
Core Design Contradiction:
Stability of the object's compositionVSReliability

Solution Approach 1:

The patent applies the extraction principle by removing water from the pyripyropene derivative to create the anhydrous Form B before formulation. This extraction of water prevents the formation of unstable hydrate forms that would otherwise occur in the presence of surfactants and moisture, thereby ensuring formulation reliability and consistent particle stability without hydrate-related issues.

Inventive Principle:
Principle #2Taking out (Extraction)

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 method produces stable aqueous suspension concentrate formulations of pyripyropene derivative I, ensuring long-term storage stability and preventing particle agglomeration, allowing for effective use as a pesticide without gelling issues.

Implementation Method 1

aqueous suspension concentrate formulations of the compound of formula I in the form of fine particles containing at least one surfactant and water

Methodology Applied
Scientific EffectSurfactant: Surfactant

Implementation Method 2

subsequent temperature-controlled processing to stabilize the formulation without converting the compound into specific hydrate forms

Methodology Applied
Scientific EffectTemperature control: Heat Treatment

Implementation Method 3

comminuting the coarse particles in the slurry of the compound of formula I to obtain an aqueous suspension of the compound of the formula I, wherein the particles of the compound of the formula I have an volume average particle size in the range from 3 to 10 μm

Methodology Applied
Scientific EffectComminution: Mechanical Force

Data Source

PatentUS10004224B2Method for producing aqueous suspension concentrate formulations
Publication Date: 2018.06.26 BASF SE

AI summary

The present invention relates to a method for producing an aqueous suspension concentrate formulation and novel suspension concentrate formulations of the compound of formula I. The method comprises the steps a) to d) as described hereinafter: a) providing an aqueous slurry of the compound of the formula I containing the compound of formula I in the form of coarse particles dispersed in a solution of the at least one surfactant in water; b) comminuting the coarse particles in the slurry of the compound of formula I to obtain an aqueous suspension of the compound of the formula I, wherein the particles of the compound of the formula I have an volume average particle size in the rage from 3 to 10 μm, as determined by light scattering; c) keeping the suspension of step b) at a temperature in the range of 20 to 95° C., d) subjecting the suspension of step c) to a further comminution to obtain an aqueous suspension of the compound of the formula I, wherein the particles of the compound of the formula I have an volume average particle size of below 3 μm, as determined by light scattering.