Preservative-Free Liquid Insulin Formulation Stability

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Solution Overview

Problem

Commercial insulin formulations face challenges with chemical and physical instability during storage and shipment, leading to degradation issues such as fibril formation and loss of potency, particularly due to the absence of preservatives and stabilizers like phenolic compounds which can be irritating.

Innovation Solution

Development of liquid insulin formulations containing 1-13 mM insulin, 50-150 mM salt, 3-24 mM pH buffering agent (citrate), and 1.9-2.7 zinc ions per insulin hexamer, without preservatives or stabilizers, optimized for pH 7.2-8.0 to maintain solubility and stability, allowing for extended shelf life and resistance to shear forces.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If phenolic preservatives and stabilizers are added to promote hexamer stability, then insulin chemical stability is improved, but patient safety and tolerability deteriorate due to mucosal irritation and malodorous effects

Engineering Contradiction:
Improveinsulin chemical stabilityVSAvoidmucosal irritation
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The invention removes phenolic preservatives and stabilizers from the insulin formulation, extracting the harmful components while maintaining insulin stability through alternative means (pH control at 7.2-8.0, zinc ions at 1.9-2.7 per hexamer, and specific ionic strength conditions). This eliminates mucosal irritation while preserving hexamer stability.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention changes the formulation parameters by controlling pH within a specific range (7.2-8.0) and adjusting zinc ion concentration (1.9-2.7 per hexamer), which stabilizes insulin through conformational changes in the B1-B8 region without requiring phenolic compounds. This parameter optimization resolves the contradiction between stability and safety.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If insulin concentration is increased to reduce formulation volume, then productivity is improved, but physical stability deteriorates due to increased susceptibility to fibril formation during shipment

Engineering Contradiction:
Improveformulation concentrationVSAvoidphysical stability
Core Design Contradiction:
ProductivityVSStability of the object's composition

Solution Approach 1:

The invention optimizes multiple parameters simultaneously: pH (7.2-8.0), zinc ion concentration (1.9-2.7 per hexamer), and ionic strength (50-150 mM salt). This combination stabilizes the hexameric form even at high insulin concentrations (up to 1000 U/mL or higher), preventing fibril formation during shipment while maintaining high productivity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention creates a composite formulation system where zinc ions, pH buffering agents, and salt components work synergistically to stabilize insulin. This composite approach allows high concentration formulations to maintain physical stability by promoting hexamer formation and preventing monomer aggregation into fibrils.

Inventive Principle:
Principle #40Composite materials

3Quantity of substance

If pH is adjusted to optimize solubility, then insulin solubility is improved, but chemical stability deteriorates due to increased deamidation reactions at higher pH

Engineering Contradiction:
Improveinsulin solubilityVSAvoidchemical stability
Core Design Contradiction:
Quantity of substanceVSReliability

Solution Approach 1:

The invention identifies an optimal pH window (7.2-8.0) that balances solubility and chemical stability. Within this range, insulin maintains adequate solubility while deamidation rates are controlled. The specific zinc ion concentration (1.9-2.7 per hexamer) further modulates this balance by stabilizing the hexameric form, which protects against pH-dependent degradation.

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 formulations demonstrate enhanced chemical and physical stability, maintaining insulin potency and solubility for at least 24 months, with reduced degradation products and improved resistance to shear forces, making them suitable for both injection and inhalation delivery.

Implementation Method 1

The binding of two zinc molecules facilitates 3 dimers (In 2 ) assembling into the hexameric form. Hexameric insulin can transition between two primary states: T 6 and R 6 .

Methodology Applied
Scientific EffectMetal coordination:

Implementation Method 2

phenolic preservatives and stabilizers bind to hydrophobic pockets located near the surfaces of insulin to promote the R 6 state

Methodology Applied
Scientific EffectHydrophobic interaction:

Implementation Method 3

The hydrophobic surfaces of the insulin molecule bind together, irreversibly forming an insulin fiber. Insulin monomers continue to bind, and the fiber elongates until it becomes insoluble in aqueous solution.

Methodology Applied
Scientific EffectHydrophobic aggregation:

Implementation Method 4

The fiber elongates until it becomes insoluble in aqueous solution. The formation of these inactive insulin fibers, results in visible cloudiness and loss of potency

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 5

a pH in the range of 7.2 to 8.0

Methodology Applied
Scientific EffectpH buffering:

Data Source

PatentEP3261648B1Liquid insulin formulations and methods relating thereto
Publication Date: 2023.12.06 AERAMI THERAPEUTICS INC
  • EP3261648B1 patent drawingFigure 1
  • EP3261648B1 patent drawingFigure 2
  • EP3261648B1 patent drawingFigure 3~4

AI summary

Liquid formulations of insulin that contain physically and chemically stable insulin but do not contain preservatives or stabilizers are provided. The formulations also lack surfactants. The formulations are useful for various modes of delivery including pulmonary delivery.