Have you validated your analytical test method used for cleaning samples?

According to the Code of Federal Regulations (21 CFR 211.67 Equipment Cleaning and Maintenance), facilities must have an effective equipment cleaning program.  Furthermore, To ensure your equipment is clean, you must verify by taking samples during the cleaning process. These sample must be tested using an analytical test method. These methods must be validated.

A company recently received the following observation:

…. Test methods used for the verification of cleaning of production equipment are not established.


a.         The firm uses unvalidated analytical test method to perform routine equipment cleaning verification. The analytical test method currently used to quantify the residual products on cleaning are tested with Thin Layer Chromatography (TLC) method. This TLC method originally developed to determine completion of … in step during manufacturing process. This TLC method has not been demonstrated to quantify to the levels of the cleaning validation requirement, detection limit of … ppm.

b.         Cleaning validation of … utilized UV-Visible Spectrometric method …. However, currently the company utilizes a TLC method for rinse sample tests for equipment cleaning verification. This method was never verified and hence no assurance that the production equipment is completely free from API or degradants as a proper analytical method is not used.

According to GMP Trends® Annual Reports, over the last 5 years the observations pertaining to equipment cleaning (21 CFR 211.67(a), and 21 CFR 211.67(b)) have been in the top 10 observations cited by the FDA each year.

For more information on FDA’s expectations regarding equipment cleaning, refer to Validation of Cleaning Processes.

To view more observations pertaining to equipment cleaning, refer to the following GMP Trends® Issues: 1111, 1096, 1052, 1033.

For more observations pertaining to manufacturing controls, see our new Issue 1116 available today.  It also has observations pertaining to quality systems, API manufacturing controls, and medical devices.

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