抽象的

Quantification of Bosantan residue on manufacturing equipment surfaces by liquid chromatographic method

K.Balamurugan, Tangirala Prakasam, K.R.Srinivasan, Thirupathi Rao, Kathirvel Asokan

Cleaning validation is an integral part of current good manufacturing practices in any pharmaceutical industry. Now a days, Bosentan monohydrate and several other pharmacologically potent pharmaceuticals are manufactured in same production area. Carefully designed cleaning validation and its evaluation can ensure that residues of Bosentan monohydrate will not carry over and cross contaminate the subsequent product. The aim of this study was to validate simple analytical method for verification of residual Bosentan monohydrate in equipments used in the production area and to confirmefficiency of cleaning procedure. The HPLCmethod was validated on a LC systemusing Cosmosil C8 (4.6mm×150 mm, 5µm) and methanol– water–acetic acid (40:60:1, v/v/v) as mobile phase at a flow rate of 1.0 mLmin- 1. UV detectionwasmade at 220 nm. The calibration curve was linear over a concentration range from2.0 to 22.0 µgmL-1 with a correlation coefficient of 0.999. The detection limit (DL) and quantitation limit (QL)were 0.08 and 0.28 µgmL-1, respectively. The intra-day and inter-day precision expressed as relative standard deviation (RSD.) were below2.0%. Themean recovery of method was 99.09%. The mean extraction-recovery from manufacturing equipmentswas 85.5%. The developedUVspectrophotometricmethod could only be used as limit method to qualify or reject cleaning procedure in production area. Nevertheless, the simplicity of spectrophotometricmethod makes it useful for routine analysis of Bosentan monohydrate residues on cleaned surface and as an alternative to proposed HPLC method.