Development and validation of UV- Spectrophotometric and RP-HPLC method for the analysis of raw material and formulations of Aceclofenac

Abstract

The purpose of the study is to develop and validate method for assay of Aceclofenac in tablet dosage forms using ultra violet spectrophotometry (UV) and high performance liquid chromatography (HPLC) techniques. A method was developed and validated for analysis of Aceclofenac using UV technique with methanol and phosphate buffer 7.4 as solvent. The HPLC analysis was conducted using two mobile phases, that is, “A” as Acetonitrile: Methanol (80:20 v/v) and “B” as Acetonitrile: methanol: NH3 solution (225:50:1 v/v/v). The method was used for assay determination for tablets dosage forms and results were found to be in compliance with official standards. Validation studies were also carried out for both methods. Linearity, LOD, single point calibration, precision and accuracy and % RSD were calculated. Aceclofenac standard was analysed with UV Spectrophotometer in the concentration ranges of 0.5-50 and 0.4-50 mg/L for each solvent and results showed good linearity with R2 = 0.9998 and 0.9999. The method was also specific that verifies the absence of interference at the max of Aceclofenac. UV analysis was precise with % RSD falling within 2% and LOD as 0.5 and 0.4 mg/L for methanol and PBS 7.4, respectively. The tablets of three brands showed assay percentages within specified limits in methanol (109.33, 103.90 and 105.61%) and PBS 7.4 (108.70, 100.69 and 106.60%). In HPLC analysis, mobile phase ‘B’ showed more sharp peaks with lesser HETP and Tf compared to mobile phase ‘A’. The method was checked for reliability and efficiency for assay and some of the parameters like height efficiency to theoretical plates (HETP), tailing factor, peak heights, peak widths along with validation studies (Linearity range 0.1-50 mg/L, specificity, precision, and limit of detection and single point calibration). The more basic mobile phase B using NH3 solution produced more sharp peaks as compared to less basic mobile phase A. Key words:  Aceclofenac, UV-Visible spectrophotometry, high performance liquid chromatography (HPLC), validation.