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Analyzing Trace-Level Impurities of a Pharmaceutical Intermediate Using ,,, an LCQ Deca Ion Trap Mass Spectrometer and the Mass Frontier ,,, Software Package

thways from virtually any proposed molecular structure. In this study, the Fragments & Mechanisms module is used to confirm the structures of three impurities associated with a key intermediate of a pharmaceutical lead.

Goal

Identification of the chemical structures of impurities associated with a key intermediate of a pharmaceutical drug lead.

Experimental Conditions

A pharmaceutical sample from Eisai Research Institute was submitted for analysis. All experiments were performed on an LCQ Deca ion trap mass spectrometer operating in the APCI mode. Separation was achieved using a Surveyor LC system equipped with an AQUASIL C18 column (250 x 2 mm) (Thermo Hypersil-Keystone). The sample was isocratically eluted off of the column using 40% water:60% acetonitrile at a flow rate of 300 L/min, without splitting.

The following source conditions were used for the LCQ Deca: Positive ionization Heated Capillary Temp: 175 C Vaporizer Temp: 325 C APCI Discharge Current: 5 A Sheath gas: 80 units Aux gas: 20 units

Mass Frontier Software

Mass Frontier provides an advanced set of analytical tools designed specifically to increase the throughput of spectral interpretation.Included among its eight modules is the Fragments & Mechanisms module that enables the automatic prediction of fragmentation pathways and reaction mechanisms from user-supplied chemical structures. Based on a mathematical approach to the simulation of unimolecular ion decomposition reactions, the Fragments & Mechanisms module contains known reaction mechanisms for molecules ionized by electron impact, protonation, and chemical ionization.


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