Thursday, December 30, 2010

Cleaning validation, stability SOP trip up API manufacturer

Industriale Chimica, Sacronno, Italy, received a two-item 483 for incomplete cleaning validation in the manufacture of active pharmaceutical ingredients (APIs).
The EIR stated that investigator Vlada Matusovsky from the Center for Drugs conducted the inspection, which covered quality, laboratory control, production, facilities and equipment systems.
Cleaning validation performed in 2003 on the manufacturing equipment used in production of several APIs was incomplete because it did not include the evaluation of effectiveness of the manufacturing equipment cleaning procedures to remove an undisclosed residue, according to the 483.
Also, the report noted that the validation did not include the determination of the existence of an undisclosed substance used by the firm to store intermediates and APIs during processing, FDA added.
According the report, management conceded, "the effectiveness of these cleaning procedures was not established with respect to their ability to remove [undisclosed substance]."
The firm further explained that the acceptance criteria for the cleaning validation was determined based on the pharmacological activity of the most and least potent products.
Then, the products were grouped into different categories depending on their solubility in the solvent used for cleaning and one product from each category was then selected as the worst-case scenario. "These products were used to evaluate the effectiveness of the cleaning procedures," the report added.
Next, the EIR stated that the SOP for long-term stability was not followed in that samples were collected outside of the specified time frame for various stability stations. It stated that stability samples were to be analyzed during the week due or in subsequent weeks.
For example, one lot initially was tested Jan. 23, 2004, while the three-month station for normal stability testing was analyzed March 4, 2004, which was more than one month early. Also, another lot initially was tested May 17, 2004, while the three-month station for normal stability testing was analyzed Oct. 4, 2004, which was more than one month later.
Industriale Chimica, Sacronno, Italy, 10/25-28/04, Doc. 109918M, $15 plus retrieval.

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