Complete Analysis cited in 9-item 483 for faulty laboratory records.

Complete Analysis Laboratories, Parsippany, NJ, received a nine-item 483 because the control testing laboratory's records did not include complete data derived from all tests, according to the report written by investigator Tara Gooen from the Parsippany, NJ, District Office.

The EIR was not available at press time.

"Raw data is missing for the gas chromatography analysis of organic volatile impurities in methscopolamine bromide 5.0 mg tablets. The certificate of analysis for sample 54147.1 for acetone and methyltbutyl ether impurities lists the data reference as chemtest book #11, page 25. However, that page is blank and the firm owner, not the performing chemist is assigned to chemtest book #11," FDA stated.

Also, the raw data in the laboratory notebook for atomic absorption analysis always was performed by the same analyst. "[It] does not document the standards used or calibration data ensuring the equipment was suitable prior to use ..." the document noted.

Further, FDA documents reported that the accuracy, sensitivity, specificity and reproducibility of test methods were not established.

"An unvalidated, undocumented, non-compendial elemental analyzer method ... was used on Jan. 9, 2006, although the certificate of analysis references the compendial method," the FDAer wrote.

In addition, an unvalidated, undocumented, modified version of a compendial gas chromatography method for a sample of ethanol content in methscopolamine bromide 5.0 mg tablets was used although the certificate of analysis references USP methods.

Next in the 483 was that the use of instruments not meeting established specifications was observed. For example, the GC atomic absorption system and elemental analyzer were not qualified or deemed suitable for use in testing of drug components, such as, sodium bicarbonate, magnesium stearate and povidone.

Further, the report stated that laboratory controls did not include the establishment of scientifically sound and appropriate standards and test procedures designed to assure that components and drug products conform to appropriate standards of identity, strength, quality and purity.

"There is no procedure or determination that the elemental analyzer, a combustions column/chromatography column unit, is suitable to analyze a sample, such as, povidone, USP for nitrogen content," the 483 noted. Standards were not run before and after analysis, but the relative standard deviation is not calculated and specifications were not established.

Also, FDA stated that the establishment of laboratory control mechanisms including any changes were not drafted by the appropriate organizational unit.

The agency stated: "The firm failed to perform and establish written procedures regarding calibration and preventative maintenance for the elemental analyzer, atomic absorption system and balances used to analyze drug components and measure samples and standards."

More specifically, calibration and preventative maintenance was not performed for the chromatography column or nebulizer in the elemental analyzer used to analyze nitrogen content in providone USP. "Maintenance was performed on Feb. 21, 2006, by an outside vendor due to the observation of unusual peak broadening and increased retention time.

"The field service report stated that several leaks were found and the septum and bymatic valve were replaced. However, the problem was not resolved until the chromatography column was replaced; no investigation was conducted and no preventative maintenance schedule was established," the FDAer wrote.

Also regarding laboratory records, FDA determined that they did not include the initials or signature of a second person showing that the original records were reviewed for accuracy, completeness and compliance with established standards.

The firm was not available for comment.

Complete Analysis Laboratories, Parsippany, NJ, 2/28-3/13/06, Doc. 115376, $5 plus retrieval.

Complete Analysis Laboratories, Parsippany, NJ, Parsippany, NJ, District