The method development process is based on a planned approach, with the first phase consisting of specification of the project goals, literature search, scientific evaluation of known data, preparation of the experimental plan and collecting all required materials. The experiments are carried out in a systematic way in order to provide a robust analytical method and to get an extensive support for the whole life cycle of the developed method.
Pre-validation experiments, including testing of the key validation parameters (precision, accuracy…), are designed and carried out in order to determine the method performance parameters, to reveal possible weak points of the method and to assure smooth progression of the subsequent validation.
A comprehensive development report, containing all relevant data and including a detailed discussion of results.
For the development of HPLC methods, we use a dedicated HPLC instrument Agilent 1260 Infinity equipped with a switching valve for up to 12 mobile phases, a column switching valve, DAD and FL detector. Different (U)HPLC systems (Agilent 1100, 1200, 1260, 1290, Waters Alliance 2695, Waters ACQUITY UPLC H-Class System) of different configuration equipped with various detectors (VWD, DAD, FLD, RI, CAD, MS) can be employed for the development.
LUNARIA’s R&D has a number of different columns dedicated to development of projects for separation of the most challenging complex mixtures.
The process of analytical method development follows modern trends of pharmaceutical analysis in accordance with the quality-by-design concept.
We offer validation of instrumental and non-instrumental analytical methods, either provided by the customer or developed in-house. Validations are performed in accordance with the ICH/VICH guidelines on validation of analytical procedures (ICH Q2(R1) guideline, VICH GL1 and GL2 guidelines).
In the first phase of the validation, a validation protocol is prepared and approved. The validation protocol contains a description of the validated method, preparation procedures for all reference and test solutions and a detailed list of validation tests together with pre-defined acceptance criteria for individual tests.
In the next phase, validation experiments are performed according to the validation plan. Any deviations or results not fulfilling the approved acceptance criteria are documented and thoroughly investigated.
The results are summarized in a validation report. It compares all validation results to the acceptance criteria and clearly concludes the suitability of the analytical method for the intended purpose.
Forced degradation studies (FDS) play an important role in evaluation of stability-indicating ability of analytical methods, investigation of degradation pathways of active substances or assessment of sensitivity of chemical substances to different conditions. In FDS, the investigated substance undergoes degradation by various physicochemical processes (influence of heat, light, humidity, oxidation, presence of acidic/ basic environment etc.) in order to degrade a pre-defined fraction of the substance.
Depending on the FDS aim, an experimental plan is prepared, defining the employed degradation conditions and analytical methods used for subsequent analysis of the degraded samples. Then a series of FDS experiments is performed according to the plan and the obtained samples are analyzed.
The results of the FDS study are summarized in the report.
LUNARIA’s R&D provides services associated with the identification of unknown impurities in pharmaceutical materials. The project typically requires employment of several analytical techniques. The selection depends on the complexity of the project and the chemical structure of the parent molecule.
Using knowledge on the studied active substance, investigation of degradation pathways using forced degradation approach is performed, in order to reveal conditions promoting the occurrence of the unknown impurity and to determine optimal degradation procedures for preparation of enriched material used for isolation of the unknown impurity by semi-preparative separation.
The determination of structure of the unknown impurity is based on results of multiple analytical techniques – mass spectrometry, NMR, UV-VIS, chromatographic behavior etc. The obtained data are combined in order to get an unambiguous assignment of the structure of the unknown impurity.
We are also able to provide the reference standard material of the impurity by preparing sufficient amount of the impurity substance with subsequent full characterization of the material to determine identity and purity of the prepared reference standard.
Determination and control of critical nutrients in cell culture is important to maximize protein yield and provide a consistent manufacturing process.
The HPLC Amino Acid Analysis Solution meets the specific demands of analyzing amino acids for protein characterization, cell culture monitoring and nutritional analysis of foods or feeds and provides accurate, high throughput amino acid analysis.
Pharmaceutical & Formulation Development of LUNARIA provides services in the field of the development of pharmaceutical dosage forms, manufacturing and analytical control for the preparation of the Registration File.
LUNARIA offers contract research services in chemical and pharmaceutical product development on pharmaceuticals, mainly generics.
LUNARIA is interested in the development of liquid dosage forms, creams, dispersions, capsules and lyophilized injections and infusions.
The health care products industry is experiencing dramatic change. The percentage of generics will stay high but they will be cheaper. In the future, our formulation laboratory will be equipped with the necessary instrumentation for the pharmaceutical development.
Biomolecules will dominate the R&D sector. Prolongation of the shelf-life of these drugs can be achieved by freeze-drying. LUNARIA therefore wants to invest in a freeze-drying equipment.