Laboratory for Chromatographic & Spectrometric Analysis

The ChromSpec Lab can rely on state-of-the-art infrastructure for carrying out research assignments and collaborations with industry and academia as part of projects and degree theses.

The key research areas include the optimisation and development of analytical methods with detection limits in the low ppb range in complex matrices and the processing and statistical analysis of measurement data. Chromatographic separation techniques are applied to quantify volatile, semi-volatile and non-volatile compounds in complex samples. The focus is on the identification, characterisation and quantification of by-products in the production of pharmaceuticals and of migrating packaging components and the characterisation of polymers.

The laboratory is equipped to handle analytical tasks in the following research areas:

• In-process purity testing and identification of impurities
• Migrating packaging components: extractables and leachables
• Method development for biomarker identification 

Impurities are components of active agents or pharmaceuticals which are chemically different from the active ingredient, the excipient or other additives. Potential sources of impurities include raw materials, solvents, intermediates, excipients and their decomposition products, which may form during production and storage.

Impurity testing, identification and quantification represent important development steps in ensuring the purity, safety and quality of pharmaceutical or food products. Specific highly sensitive methods are required to detect, isolate and qualify these impurities, which are often present in very small amounts and in complex sample matrices.

Better insight into the active ingredient and the pharmaceutical product as also their development at laboratory scale through to upscaling processes enables even complex production processes to be addressed in an ever stricter regulatory environment. These questions can be addressed by studies with a high level of analytical expertise and robust analytical results.

The scientists at the ChromSpec Lab adapt and develop analytical methods to identify and quantify these unknown substances. They use stability studies to simulate degradation processes and to identify and quantify potentially harmful compounds.

Structural characterisation is carried out using different ionisation techniques (EI, CI, ESI, APCI) for GC and LC mass spectrometry and a two-dimensional chromatography system in comprehensive and multiple heart-cutting mode.

Components of primary packaging materials and medicinal products can migrate into the packaged product or metabolically interact with product components. Assessing and mitigating the risk of extractables and leachables from packaging materials for foods and medicines poses a substantial challenge to supervisory authorities and manufacturers. A comprehensive analysis includes the identification and quantification of these components, taking into account the adverse biological effects of the individual chemical structures. Compounds such as softeners or other polymer additives used in the manufacture of polymer-based packaging material are endocrine disruptors suspected of influencing the human immune system and thus the regulatory processes in the body.

A multi-dimensional screening model was developed to investigate the migration and bioactive potential of these sensitive and unstable substances. When combined with selective and quantitative detection techniques, this model allows volatile, semi-volatile and non-volatile compounds to be detected and provides information about the chemical and immunomodulatory properties of the substances detected in vitro.

The ChromSpecLab offers support in optimising holistic analytical processes using GC-MS/MS and LC-MS/MS methods, from experimental design (e.g. study design, sample preparation, extraction), choice of the analytical setup and adaptation of device-specific parameters through to data processing and statistical analysis.

The team of experienced specialists can draw on an extensive infrastructure including a range of GC/MS and LC/MS systems:

Gas chromatography – mass spectrometry:

• Agilent 7890B GC with Agilent 7010C Triple Quadrupole MS with EI/NCI ionisation
• PAL 3 RSI Autosampler with headspace, SPME and injection module
• Agilent 7890B GC with Agilent 5977B Single Quadrupole MS with EI/NCI ionisation
• Agilent 6890 GC with Agilent 5975 Single Quadrupole MS and 7697A Headspace Sampler
• Agilent 6890 GC-FID with 7697A Headspace Sampler

Liquid chromatography – mass spectrometry

• Agilent 6460 Triple Quadrupole MS with ESI/APCI ionisation
• Agilent 1290 Infinity II 2D-UHLC System
• Agilent 1290 Infinity UHPLC System
• Agilent 1290 Infinity II Evaporative Light Scattering Detector
• Agilent 1260 Infinity UHPLC System with Fraction Collector
• Thermo LCQ Fleet
• UHPLC Accela 1000