Headspace Oxygen Analysis

Method Introduction

Headspace oxygen analysis (HOA), also known as Frequency Modulation Spectroscopy (FMS), is a noninvasive technique for determining the oxygen content in the headspace of a freeze-dried drug product.

HOA measures the absorption of laser light with a wavelength of 762 nm that passes through the gaseous headspace of a vial containing the freeze-dried drug product. The oxygen content in the headspace is determined using a calibration curve from standards of known oxygen concentrations. Since absorption is dependent on the path length and influenced by the optical properties of the container, container-specific standards are constructed.

Applications

HOA can be used during lyophilization process development, stability studies, and quality control testing of freeze-dried products. A consistently low headspace oxygen content is important for determining container closure integrity. Further, changes in headspace oxygen content can indicate drug product instability, such as oxidation-related protein degradation.

A significant benefit of HOA is its non-destructive nature, allowing for 100% testing of drug products or a subsequent analysis of the same vial using other techniques. Further, the analysis time is short, and its performance is straightforward. HOA, however, requires a rather elaborate method of development using standards in the respective container, making it less attractive for early-stage lyophilization/formulation development and individual sample testing.

Quality and Biosafety Level

We provide all our analytical services with the highest quality standards. Experienced scientists carry out each project, and a scientific reviewer comprehensively checks every report or data presentation.

We offer this technology with the following quality and biosafety levels:

R&D level

We offer this method under R&D. Our GRP system assures the highest-quality research standards.

Up to biosafety level 2

This method can be applied to nucleic acids, viruses, cells, viral vectors, including lentiviruses and more.

Analytical Method Development, Qualification and Validation

For common sample types, we can often apply standardized methods with little setup effort. However, when needed, our experienced analytical experts create or optimize custom methods tailored to your active pharmaceutical ingredient, product type and development phase.

Method Development

Our method development approach tailors sample preparation, method settings and data analysis to the needs of your project and sample.

We include representative samples and, where available, suitable reference standards and stressed/degraded materials, allowing our analytical scientists to design a highly suitable, stability-indicating, robust and repeatable method. Upon request, we will compile a detailed description of the method for your records.

Method Qualification

Method qualification is the initial assessment of an analytical procedure’s performance to show its suitability for its intended purpose.

During method qualification, our analytical scientists perform documented testing demonstrating that the analytical procedure meets criteria in several categories. Criteria may include factors such as repeatability, specificity and robustness. We compile a qualification plan and report, including all relevant data.

Method Validation

Under GMP conditions, method validation confirms that an analytical procedure’s performance suits its intended purpose. Depending on the method’s scope, a broad range of method characteristics, such as specificity, accuracy, precision, limit of detection/limit of quantification (LOD/LOQ), linearity and range, is considered.

During method validation, our analytical scientists perform documented testing demonstrating that the analytical procedure consistently produces a result that meets the predetermined acceptance criteria. We compile a validation plan and report that includes all relevant data.

Depending on the development phase, a fit-for-purpose validation approach can be offered, adjusting the validation required efforts in a phase-appropriate way to meet the method’s needs.

Method Verification

Compendial method verification confirms that a compendial method (e.g., from Ph. Eur. or USP) is suitable and reliable for its intended purpose under the specific conditions of the laboratory.

Unlike full method validation, compendial method verification is often considered a partial validation since the method has already undergone extensive testing and validation during its inclusion in the compendium. The extent of method verification depends on the type of method.

During method verification, our analytical scientists perform documented testing demonstrating that the developed analytical method performs adequately for the specific product or matrix being tested and within the specific laboratory where the method will be employed.

Talk to Our Experts or Request a Quote

Our expert team is ready to answer your questions and guide you to the services best suited to your program’s modality, stage and challenge. If your needs are well-defined, we’ll begin the quotation process.

Related Services

Headspace moisture analysis (HMA) Freeze-drying microscopy (FDM) Differential scanning calorimetry (DSC) Karl-Fischer titration (KFT) Gas adsorption analysis based on the Brunauer–Emmett–Teller (BET) theory X-ray powder diffraction (XRD)

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