Agenda1 were approached by an overseas client and asked to assist with their development of an amorphous API. Communication routes were established via email and telecom with the project being defined via a series of telecom “meetings”. Timelines were agreed for shipping of materials and delivery of data which proved to be achievable, and faster than available locally to the client.
The client was developing a process for the manufacture of an amorphous API and had identified the SSA (Specific Surface Area) as a key product performance feature. Part of the process development process involved a DOE (Design of Experiments) programmes. This generated large numbers of samples for analysis. The analytical data had to be of suitable quality to support a potential regulatory submission in the future, and had to be available quickly to allow testing of changes to the manufacturing parameters as felt appropriate.
Agenda1 were selected by the client as they were unsatisfied with their local turnaround which failed to meet their timeline requirements. The client needed a cost effective method that would provide results within five days from the sample receipt. In addition to the routine analysis, Agenda1 were also asked to collate raw data packages, summary reports for the DOE work and to carry out other analysis work such as Helium Pycnometry.
Using their in house equipment and their team of skilled scientists, Agenda1 developed a client specific method that could produce accurate results within the client’s timeline. This involved testing a range of different sample preparation approaches and run times to both produce good data and meet the tight timelines.
The team used a Micromeritics TriStar3000 Surface Area Analyser apparatus and flow prep system, this set up allowed the simultaneous analysis of three samples in a single run, the analysis of samples being carried out in parallel to the sample prep to facilitate fast turnaround.
In carrying out this work, the prior Agenda1 knowledge of and experience with amorphous materials was critical in ensuring the data could be relied upon.
A glove box was used to handle the materials as they were humidity sensitive and required low humidity conditions.
Agenda1 developed an instrument performance protocol in conjunction with the analytical method to certify the approach was suitable for use before committing samples to analysis. To ensure appropriate resources were available, additional analysts were trained .
SSA was determined by BET nitrogen adsorption. The analytical procedure was approved by the client and was in place to ensure consistent analysis of the samples.
Samples were sent on out by the client on a Friday and received by Agenda1 on the following Monday with analysis commencing promptly, data being provided by the following Thursday, 6 days after shipping.
A report summarising all data was assembled for the client. The client also required hard copies of the data for PDF archiving and these too were provided. Work was carried out in timetable to meet the client needs, and distance proved little obstacle to effective working.