Alkaline Crystallization of Insulin Glargine

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Solution Overview

Problem

Current methods for crystallizing insulin glargine are often performed at a pH slightly above or less than the isoelectric point (pI) of the insulin, resulting in small crystals that are difficult to separate efficiently, whereas there is a need for alternative methods to produce larger, ordered crystals of insulin glargine.

Innovation Solution

Crystallizing insulin glargine at a pH at least one or more units greater than its pI, using a solution with isopropanol, meta-cresol, and ammonium acetate, and adding zinc chloride to induce crystallization, allowing the crystals to settle and be filtered and dried in a filter apparatus to produce large, ordered crystals greater than 10 µm in size.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If insulin glargine is crystallized at a pH slightly above or less than the isoelectric point (pI), then the crystallization process is conventional and manageable, but the resulting crystals are small and difficult to separate efficiently

Engineering Contradiction:
Improvecrystallization process managementVSAvoidcrystal separation efficiency
Core Design Contradiction:
Ease of operationVSProductivity

Solution Approach 1:

The patent applies parameter changes by shifting the pH condition from the conventional range (slightly above or below pI) to a significantly alkaline range (at least one pH unit greater than pI, specifically pH 9.0-10.0). This parameter change transforms the crystallization outcome from small, difficult-to-separate crystals to large, filterable crystals with average size greater than 10 µm, thereby resolving the contradiction between process manageability and separation efficiency

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If insulin glargine is crystallized at a pH at least one unit greater than pI, then large ordered crystals greater than 10 µm are produced, but the crystallization requires alkaline conditions (pH 9.0-10.0) which is a departure from conventional methods

Engineering Contradiction:
Improvecrystal size and orderVSAvoidpH condition flexibility
Core Design Contradiction:
Manufacturing precisionVSAdaptability or versatility

Solution Approach 1:

The patent employs parameter changes by establishing specific alkaline pH conditions (pH 9.0-10.0, at least one unit greater than pI) that enable the formation of large, ordered crystals with average size greater than 10 µm. This controlled parameter change achieves high manufacturing precision for crystal size and order, resolving the contradiction between crystal quality and pH condition flexibility

Inventive Principle:
Principle #35Parameter changes

3Productivity

If zinc chloride is added to induce crystallization, then crystallization is promoted and crystals form, but the addition of zinc chloride requires precise concentration control (13.2-16.8 mg per gram of insulin glargine)

Engineering Contradiction:
Improvecrystallization rateVSAvoidzinc chloride concentration control
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent applies parameter changes by optimizing the zinc chloride concentration to a specific range (13.2-16.8 mg per gram of insulin glargine) that simultaneously achieves high crystallization productivity and maintains precise manufacturing control. This optimized parameter setting resolves the contradiction between promoting rapid crystallization and maintaining precise concentration control

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

This method enables the production of large, ordered insulin glargine crystals with an average size greater than 10 µm, achieving high purity and yield, and allowing for efficient separation and drying, overcoming the limitations of existing methods.

Implementation Method 1

adding zinc chloride to the solution and incubating the solution at a temperature of 17°C to 23°C with agitation for four to eight hours for the insulin glargine to crystalize and produce the insulin glargine crystals

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 2

allowing the crystals to settle and be filtered

Methodology Applied
Scientific EffectSedimentation: Sedimentation

Data Source

PatentEP3077414B1Method for preparing crystalline insulin
Publication Date: 2020.06.17 MERCK SHARP & DOHME CORP
  • EP3077414B1 patent drawingFigure 1A
  • EP3077414B1 patent drawingFigure 1B
  • EP3077414B1 patent drawing

AI summary

A method for crystallizing insulin or insulin analogs under alkaline conditions and purifying the insulin or insulin analog crystals by filtering through a filter and drying the insulin or insulin analog crystals captured on the filter to produce crystalline insulin or insulin analog crystal compositions is described. In particular aspects, the method may be used to crystalize insulin glargine.