Polysorbate Quantification via ATR-FTIR Internal Standard

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Solution Overview

Problem

Existing methods for quantifying polysorbates, such as polysorbate 80, in complex mixtures face interference from matrix constituents, requiring complex and time-consuming sample preparation, and lack sensitivity and specificity.

Innovation Solution

A method using Attenuated Total Reflectance-Fourier Transform Infrared spectroscopy (ATR-FTIR) that involves obtaining a mid-infrared spectrum of a test sample with an internal standard, identifying specific peaks, and comparing normalized peak areas to a calibration curve to determine polysorbate concentration without prior chemical pretreatment of the sample.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional methods (colorimetry, HPLC, GC, GC-MS) are used to quantify polysorbates, then quantification can be achieved, but matrix interference occurs requiring complex and time-consuming sample preparation

Engineering Contradiction:
Improvequantification accuracyVSAvoidsample preparation complexity
Core Design Contradiction:
Measurement precisionVSDevice complexity

Solution Approach 1:

The patent extracts only the essential spectral information needed for quantification by using ATR-FTIR to directly measure the carbonyl peak area ratio between polysorbate and internal standard, eliminating the need for complex sample preparation steps such as extraction, derivatization, or separation that are required by conventional methods

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent introduces an internal standard (azide) as an intermediary substance that does not interfere with the polysorbate measurement but provides a reference peak for normalization, thereby compensating for matrix effects and eliminating the need for complex sample preparation while maintaining quantification accuracy

Inventive Principle:
Principle #24Intermediary (Mediator)

2Measurement precision

If conventional methods are used for polysorbate quantification, then concentration can be determined, but the process is time-consuming due to complex preparation

Engineering Contradiction:
Improveconcentration determination accuracyVSAvoidsample preparation time
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent extracts only the essential spectral information needed for quantification by using ATR-FTIR to directly measure the carbonyl peak area ratio between polysorbate and internal standard, eliminating the need for complex sample preparation steps such as extraction, derivatization, or separation that are required by conventional methods

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The method enables direct measurement of polysorbate concentration in complex matrices without requiring external sample preparation interventions. The ATR-FTIR technique with internal standard normalization allows the system to self-correct for matrix effects, eliminating time-consuming preparation steps while maintaining accuracy

Inventive Principle:
Principle #25Self-service

3Quantity of substance

If conventional test methods are used, then polysorbate concentration can be measured, but sensitivity and specificity are insufficient due to matrix interference

Engineering Contradiction:
Improvepolysorbate concentration measurementVSAvoidsensitivity and specificity
Core Design Contradiction:
Quantity of substanceVSReliability

Solution Approach 1:

The patent introduces an internal standard (azide) as an intermediary substance that does not interfere with the polysorbate measurement but provides a reference peak for normalization, thereby compensating for matrix effects and eliminating the need for complex sample preparation while maintaining quantification accuracy

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent changes the measurement parameter from absolute peak area to normalized peak area ratio (polysorbate carbonyl peak area divided by internal standard peak area), which transforms the measurement into a relative quantity that is insensitive to matrix effects, thereby improving sensitivity and specificity

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 approach allows for accurate and efficient quantification of polysorbate 80 in complex formulations, including vaccine components, without interference from the matrix, and demonstrates high sensitivity and specificity, as confirmed by GC-MS results.

Implementation Method 1

obtaining a mid-infrared Attenuated Total Reflectance (ATR) spectrum of the test sample

Methodology Applied
Scientific EffectAttenuated Total Reflectance: Total Internal Reflection

Implementation Method 2

Attenuated Total Reflectance-Fourier Transform Infrared spectroscopy (ATR-FTIR)

Methodology Applied
Scientific EffectFourier Transform Infrared spectroscopy: Absorption Spectroscopy

Data Source

PatentEP2852828B1Method for determining a concentration of a polysorbate species in a mixture
Publication Date: 2016.04.06 GLAXOSMITHKLINE BIOLOGICALS SA
  • EP2852828B1 patent drawingFigure 1
  • EP2852828B1 patent drawingFigure 2
  • EP2852828B1 patent drawingFigure 3

AI summary

A method for determining a concentration of a polysorbate species, such as polysorbate 20, polysorbate 40, polysorbate 60, or polysorbate 80, in a mixture comprises obtaining a test sample of said mixture, adding an internal standard, preferably azide, to said test sample, obtaining, with a spectrometer, a mid-infrared Attenuated Total Reflectance (ATR) spectrum of the test sample, e.g. by using and ATR-FTIR apparatus, identifying, from the reflectance spectrum, a wavenumber corresponding to the C=0 peak (e. g., 1735 cm-1), identifying, from the reflectance spectrum, a wavenumber corresponding to the internal standard, calculating the area under the curve for said C=O wavenumber, normalized by the internal standard, and comparing said area to a calibration curve to determine the concentration of polysorbate in said test sample.