Contract Research and Services
The Centre houses an impressive range of sophisticated analytical instrumentation allowing us to offer a broad spectrum of solutions to resolve any problem. Our dedicated analytical experts have many years experience working with a range of techniques allowing them to be innovative when developing products and troubleshooting commercial challenges. The Centre has an excellent record of delivering projects on time and in full, at a competitive price.
We pride ourselves on our ability to solve problems through analytical science, no matter how small or large your challenge, please contact us to discuss how we can help.
Analytical Method Development and Validation
One of the core strengths of the Centre is our ability to develop and validate both routine and novel analytical methodologies. As an example of a routine development exercise we can develop HPLC methods for API’s that will measure %w/w assay and impurity content as described by the ICH guidelines.
We can apply a number of different detection systems including -UV (VWD and PDA), -MSn, RI, Fluorescence and ELSD. Typically, method development and validation will involve a number of steps that will start with optimising specificity, development of a stability indicating method with validation as appropriate (accuracy, precision (repeatability & reproducibility), range, linearity, robustness etc.).
Preformulation studies have a significant part to play in anticipating formulation problems and identifying logical paths in both liquid and solid dosage form development. The Centre offers a complete preformulation analytical package that is tailored to the requirements of the client.
Typically, our preformulation analytical package can include any of the following:
- Solubility (aqueous, solvent and biorelevant media), pKa, logP/D;
- Moisture content, sorption analysis;
- Thermal analysis (thermal behaviour, melting point);
- Structural characterization; FTIR, UV/Vis, fluorescence, NMR, MSn;
- Particle morphology, size and size distribution;
- Polymorph and salt screening;
- Solid state and solution stability;
- Drug-excipient compatibility and packaging component compatibility.
Deformulation is an analytical approach that deconstructs a product into its constituent components. Complete deformulation analysis can lead to a thorough understanding of the product. In general, deformulation is applied to product development and benchmarking, including competitor product analysis.
Typically, studies involve developing a broad range of analytical methods together with appropriate extraction and separation methods to identify and then quantify the components of a complex formulation.
Our analysts will use all the information available on the formulation to help us to undertake the deformulation more effectively, this can include a thorough literature search.
Deformulation may be a full quantitative description of all components or a semi-quantitative identification of the major and minor components, such that their chemical moiety and function in the formulation can be identified.
We have a great deal of experience of working with many different formulation types across multiple sectors including pharmaceutical applications (topically applied gels, creams, ointments and lotions), personal care (mouthwashes, creams, make-up products) and even sports performance enhancers.
Raman Mapping of Product Formulations
Researchers at the University of Bradford have been at the forefront of innovation in applications of Raman Spectroscopy. Our commercial team has the opportunity to work closely with leading academics to develop new or current methodologies to help resolve your challenges.
Raman Spectroscopy provides a “chemical fingerprint” of a pharmaceutical compound making it a powerful analytical tool for determining molecular composition and structure, identifying solid form (polymorphs, solvates, amorphous form) and assessing other physico-chemical properties that are important for understanding, predicting and controlling drug product performance.
Pharmaceutical Raman Imaging
The Centre has extensive knowledge and experience of using Raman Microscopy to evaluate the physico-chemical properties of pharmaceutical materials. Using 2-dimensional Raman mapping techniques the Centre have previously studied:
- Differences in physical form in pharmaceutical formulations; crystalline vs. amorphous form, polymorph identity, solvated species, co-crystal forms etc.;
- The distribution of one or more active ingredients in a pharmaceutical product, and even distribution of different forms of materials in formulations;
- The PSD of one or more active ingredients in a pharmaceutical product.
Here at the Centre we have the expertise and equipment to effectively isolate and identify both small molecule and biological unknowns/impurities and determine their source. Typically, we would use Chromatographic and Mass Spectrometry techniques to initially identify the unknown. Depending on the results we can then use a number of isolation and purification techniques to obtain sufficient quantities of purified material to allow for a more accurate characterization using remote techniques such as NMR and Vibrational Spectroscopy. We can isolate and purify the unknown using a range of techniques including:
- hydrolysis (digestion);
- liquid- liquid extraction;
- solid phase extraction;
- supercritical fluid extraction;
- preparative HPLC;
- column chromatography;
We also have the ability to synthesise small quantities of the unknown using established literature methods or by design of bespoke approaches accessing the University's experienced organic chemists. Preparation of purified, fully characterised reference materials allows unequivocal identity of impurities and generation of reference materials for future analysis.
Impactor studies for Inhaled Therapies
The Centre offers a range of services for preclinical inhaled delivery development including development and testing of DPI, pMDI and nebulised formulations.
Nebulisation allows fit for purpose formulations to be developed rapidly for use in preclinical and early clinical studies
Our structured approach to Nebulised formulation development includes:
- Selection of nebuliser devices for the study;
- Analytical method transfer or development as necessary;
- Next Generation Impactor Testing (low flow (15 L/min), refrigerated)
- Aerosol output study;
- Variation in concentration and excipient inclusion studies;
- Solution stability testing.
The Dry Powder Inhaler (DPI) is rapidly becoming popular as it reduces issues of coordination and high plume velocity without requiring large spacers or holding chambers.
Our structured approach to DPI formulation development and testing includes:
- API micronisation and associated analysis (PSD, morphology, surface energy);
- Blending studies (carrier selection, blend uniformity testing, product assessment (morphology, distribution on carrier etc.));
- Aerodynamic assessment (NGI/ACI tests for MMAD, GSD, FPD/FPF);
- Stability testing of micronised and blended API;
- Aerodynamic assessment of stored materials.
- Pressure drop measurements for device assessment.
pMDI devices are also common in the delivery of drugs to the lung. Formulation of APIs in fluorinated propellants (HFAs 134a and 227) can be performed with our partner organisations, and aerodynamic assessment on novel or commercially available products undertaken in house using impaction techniques.
- Aerodynamic assessment at appropriate flow rates (NGI/ACI tests for MMAD, GSD, FPD/FPF);
- Stability testing of products (creaming, flocculation, Ostwald ripening).
We also offer some novel, bespoke analytical methods in the area of inhaled product testing. We developed a pressurised NMR method of assessing solubility of API / excipients in volatile fluorinated propellants; HFAs134a and 227. These measurements can be crucial in predicting the stability of formulations in pMDI devices. We can also assess solid form of materials delivered from pMDI/DPI devices using microscopic, spectroscopic, thermal and diffraction methods on material collected from impaction studies. Please contact us to discuss these methods in more detail.
We provide Basic ID information for substances (main components, essential additives and impurities) such as:
- Public Name, Trade Names, CAS name and number;
- Chemical Name in IUPAC Nomenclature, EINECS/ELINCS number;
- Molecular and structural formula, including SMILES notation;
- A series of initial Analytical testing that we can perform using our on-site instrumentation such as;
- Basic spectral data acquisition using NMR, IR and UV-Vis methods;
- Stereochemistry-identifying specific optical/geometric isomers;
- Mineral identification-Spectral fingerprints;
- Fully interpreted spectra and chromatograms.
We provide the Sameness Package in which we can provide the following:
- Basic ID information on main components, essential additives and impurities;
- Basic spectral data acquisition for characterisation;
- The purity of a substance: classified under REACH as a chemical purity, a chiral purity or any essential additives within the substance;
- The composition of a substance including an estimate of the % of the total for each component in multi-component substances;
- Identification of impurities and typical % values in terms of w/w of substance;
- Fully interpreted data and comparison to database standards.
Skin Applications Analysis
The University of Bradford has for many years been a leading contributor of research into analysis of skin samples using Raman Spectroscopy. We offer services for development and implementation of Raman spectroscopic methodology for determining levels of active ingredients and distribution / penetration in skin samples.
We have worked on a number of projects using three-dimensional mapping techniques to investigate active concentration depth profiling in applied skin samples. The Centre has close links with the “Centre for Skin Science” and “Ethical Tissue Ltd” at the University of Bradford. We can obtain skin samples from Ethical Tissue Ltd located at the University of Bradford
Key active areas
- In vivo analysis of skin composition;
- Study penetration and transdermal delivery of topically applied compounds;
- Quantification of active ingredients in the skin.
- Analysis of inorganics in skin and mummification residues (archaeological application);
- In vitro DMSO treatment stratum corneum;
- Distribution of 'actives' applied from UV blocking creams (sun-creams);
- Assessment of moisture levels and levels of desiccation pre- and post- moisturiser treatment.