Agenda1 were selected by the client to assist them with the analysis of their product to develop and validate a method for quantitative metals analysis by ICP-OES in accordance with USP 232 and 233.
The client is an international company supplying high quality drug products. In this industry the cost of manufacturing drug products which fail to meet elemental impurity level requirements could be financially catastrophic to the drug product supplier. Agenda1 developed a client specific method using in house equipment and an experienced team of analysts to meet the client’s needs and help them adhere to the requirements of their key risk-based control system. The analytical work produced was in challenging circumstances has been instrumental in guiding changes to the client’s manufacturing process and helped them develop an improved product.
The pharmaceutical industry is facing changes to the techniques which will be deemed appropriate for analysing the level of elemental impurities with quantitative ICP-OES analysis favoured over old fashioned colour-change analysis. The client, an established pharmaceutical manufacturer, approached Agenda1 to develop and validate a method capable of the quantitative analysis of the four key heavy metal elements outlined in USP 232, Arsenic, Cadmium, Mercury and Lead. Agenda1 were able use their experience to help the client develop specifications for elemental impurities in their products. The experienced analytical team at Agenda1 were able to develop and validate a method that was specific for the client’s formulation, whilst overcoming a challenging sample with the addition of matrix matching. A cost effective and fast method was developed to meet the client’s requirements. Working closely with the client, Agenda1 analysed samples to a tight timeline. All work was carried out using Agenda 1’s in house equipment operated by team of skilled analysts within the time line demanded by the client.
All experimental methods are carried out by a skilled team of analysts using equipment that is regulated to GMP standards. To prepare the sample before being analysed, an Analytix Ethos UP Microwave Digestion Unit was used. The equipment suitably digested a challenging sample. The testing was carried out using the Thermo-Scientific iCAP6500 Series ICP spectrometer.
Agenda1 developed a detailed client specific method which was optimized to ensure accurate and consistent results were obtained. The experimental method development work included assessment of precision work and how reproducible the method was.
The experienced analytical team at Agenda1 were able to overcome a number of challenges during the method development stage. The challenging sample type required an alternation of the digestion method to include the addition of an alternative acid, and a higher microwave digestion temperature.
The sample was subsequently found exhibit a very high level of an alternative element which was not being analysed. The alternative element produced interference when analysing the target elements, and the internal standard element. The level of the alternative element was established, and the calibration standards were then produced with a matrix matched approach. This addition to the method allowed for the samples to be analysed successfully.
For the method development and validation a formal report was produced. This report explained the areas in which the method had been modified during the development process and detailed the results of the method validation, including the observations and recommendations of the experienced analysts at Agenda1.
The main aim of this experimental development was to achieve a method suitable for the routine analysis of client samples for release testing. The client was satisfied with the completed work and began shipping samples for routine analysis.