Development of a Cleaning Validation Protocol for an Odd Case Scenario and Determination of Methoprene residues in a Pharmaceutical Manufacturing Equipment Surfaces by using a Validated UFLC Method

Abstract

In veterinary pharmaceutical industries, it is very important to remove drug residues from the equipment and areas used for the manufacturing of a product. At the same, the associated cleaning procedures must be validated. In the present report, initially a protocol was developed to determine the Maximum Allowable Carryover (MAC) of methoprene based on an odd case scenario. A rapid, sensitive and specific reverse phase ultra-fast liquid chromatographic (UFLC) method was developed and validated for the quantitative determination of methoprene in cleaning validation swab samples. According to developed protocol, the MAC was found to be 1.068 µg/cm2. Cotton swabs, moisten with extraction solution (100% methanol) were used to remove any residue of drug from stainless steel, glass and silica surfaces and give recoveries >80% at three concentration levels. The precision of the results, reported as the relative standard deviation, were below 2.5%. The calibration curve was linear over a concentration range from 0.15625 to 5.0 µg/ml with a correlation coefficient of 1. The method was validated over a concentration range of 0.15625–5.0 µg/ml. The developed method was validated with respect to specificity, linearity, accuracy, precision, and robustness.