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May 31-June 4, 2020
George R. Brown Convention Center, Houston, TX, USA


Comprehensive Degradant Identification and Management of Analytical Data in Drug Product Development
Joe DiMartino

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Comprehensive Degradant Identification and Management of Analytical Data in Drug Product Development
Joe DiMartino

During drug product development, a large amount of time and effort is spent on chromatographic method development. Forced degradation studies (or stress tests) are carried out to build the stability indicating method. Efficient development of this method requires a complete understanding of the manufacturing process and open communication between various interrelated departments—from process chemistry through to analytical R&D.

Theoretical degradants are used by scientists for targeted analysis in forced degradation studies. Often this vital chemical information is disconnected from observed degradant data making the identification of impurities and degradants challenging and thereby slowing down the process.

Analytical data assembled for Agomelatine, synthesized following a five-stage process route, was used in this work. The data was collected on an Agilent-1200-Series with an Agilent VWD-G1314B UV detector, acquiring spectra at 210 nm, and an Agilent 6110 Quadrupole API-ESI Mass Spectrometer, collecting low resolution spectra in a 45-1000 Da mass range. Column separation was performed via an isocratic method using an ammonium formate Buffer H of 4.5/ACN (35:65). The flow rate was 1.2 mL/min with a run time of 50 min, and the column used was a Zorbax Eclipse XDB C18 5 µm – 4.6 x 150 mm. The software application Luminata® (v2019.2), based on the ACD/Spectrus Platform, was utilized to manage analytical and chemical data for the process.

Preliminary Data
In this poster we will present software tools that manage structural, analytical, and all process related data into a structured and searchable manner to facilitate inter- and intra- departmental communications. Luminata® intelligently links chemical information with related live analytical data. The tools take a theoretical degradant targeted list and batch process the mass spectrometry data automatically. Once completed, a degradant map is generated, and all related mass spectra are associated to each degradant in the map. The software also captures both observed and theoretical degradants (structures and meta data from predicted third party software) in the same interface.

Novel Aspect
Luminata enhances stability-indicating method development by analyzing stress test data in a single application and identifying degradants more efficiently.