A high performance liquid chromatography (HPLC) method with a Corona Charged Aerosol detector for the cleaning validation of MICRO* A07 Citric Acid Cleaner residue has been developed. The pooled average repeatability of 3 replicates at 6 concentration levels expressed as RSD was 1.3 % while the pooled average intermediate precision (intra-day repeatability in 3 days) of 3 replicates at 6 concentration levels was 2.4 %. Simulated maximum allowable carryover (MAC) was calculated by using 10 ppm of MICRO® A07 Citric Acid Cleaner in a tablet of 1000 mg. With this MAC value, the amount of MICRO® A07 Citric Acid Cleaner applied to a stainless steel surface was calculated. The swabbed MICRO® A07 Citric Acid Cleaner samples were quantified by this HPLC-CAD method and the average recovery of 5 replicates of swabbed samples from stainless steel surfaces was about 92 % ± 2%. The accuracy of the method was expressed as correlation coefficient, which was 99.7% by using all 3 sets of 3 replicates at 6 concentration levels in 3 days. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 60 ng and 189 ng, respectively, by using the three times and ten times standard deviation of a matrix blank run. The value of LOD was verified by running a real sample. Specificity of the method was evaluated by conducting separation of blanks, the samples matrix, and placebos (common drug excipients) plus recovery sample mixture spiked with MICRO® A07 Citric Acid Cleaner. The result shows good resolution and absence of interference to the targeted peaks from the matrices and placebos. This method is designed for use in Food and Drug Administration (FDA) regulated establishments in compliance with good manufacturing practice (GMP).
Keywords: Cleaning validation; MICRO® A07 Citric Acid Cleaner; Detergent; HPLCCAD; Maximum allowable carryover, Good manufacturing practice