Determination of Acceptable Residual Limit by Using Newly Developed and Validated RP-HPLC Method for Citalopram Hydrobromide Residues that Swabbed from Surfaces of Pharmaceutical Manufacturing Equipment

Abstract

In this study, easy and robust RP-HPLC method was developed and validated to determine acceptable residual limit of citalopram hydrobromide for cleaning procedures. The United States, Food and Drug Administration has mentioned that the acceptable limit for residues present in the equipment during processing or manufacturing should be based on logical criteria. In present study, acceptable residual limit for cleaning procedure of citalopram hydrobromide was calculated by using three approaches including therapeutic dose method, 10 ppm criteria and visual limit of inspection. The value by erapeutic dose approach was less among three calculated values hence, selected as acceptable residual limit (10.66 µg/25 cm2 ) for analytical method development and validation for the detection of this drug residues on the surfaces of manufacturing equipment. A RP-HPLC assay method was developed using C18 column and mobile phase containing mixture of methanol and ammonium acetate buffer (pH4.6) (70:30) with flow rate of 1.6 ml/min. System suitability parameters like theoretical plates and tailing factor were calculated for the validation of the developed method as per ICH Q2B guidelines. After analyzing recovery study data, it was found that stainless steel plate has minimum recovery (88.87%) and pre-analyzed tablet solution has maximum recovery (99.29%)