Development of stability indicating liquid chromatography-mass tandem spectrometric method for the estimation of mycophenolate mofetil in bulk and pharmaceutical formulations

Abstract

Aim

To develop a simple LC/MS/MS method for the determination of mycophenolate mofetil in bulk and pharmaceutical formulations and study of stability of the drug in different stressed conditions.

Methods and materials

The LC/MS/MS analysis was carried out on Applied Biosystems API 3200 triple quadrupole mass spectrometer attached to Shimadzu LC 10 AT VP series HPLC system using chromosil ODS-3, C18, 4.6 × 50 mm, 2.5 μm column. The mass spectral analysis was carried out by direct infusion of 10 μg/mL solution into the ESI source at a flow rate of 10 μL/min along with the mobile phase flow rate of 600 μL/min. All chemicals and reagents were of either analytical grade or chromatographic grade.

Results

The obtained mass spectrum showed m/z 434 as a major ion which can be attributed to the MH⁺ ion of the analyte. This ion was subjected to collision induced dissociation (CID) using nitrogen as a collision gas. The collision energy was tuned in such a way that the intensity of MH⁺ ion was reduced to a minimum of 20%. The obtained mass spectrum after CID showed m/z 114 as a major fragment. Hence the transition m/z 434 → 114 was used to monitor the analyte peak in LC/MS/MS analysis. The developed method was validated in terms of precision, accuracy, linearity, robustness and ruggedness.

Conclusions

The developed method was found to be simple, rapid, repeatable, reproducible, robust, rugged and economic hence it can be used as a new analytical method for the analysis of pharmaceutical formulations in any pharmaceutical industries.