A QC analyst injected eleven identically or similarly named samples for impurity and assay analysis approximately one to fifteen seconds apart from one another, according to the HPLC audit trail for [redacted] DMF submission batches [redacted] and [redacted]. A second analyst injected eight similarly named impurity and assay samples approximately twelve to sixteen seconds apart, according to the HPLC audit trail for the analysis of [redacted] batches [redacted] and [redacted].
Neither analyst reported all results obtained during testing. The laboratory incident reports concluded the first analyst deleted 28 original files due to pressure fluctuations and ghost peaks, while the second analyst deleted original trial injections of working standard and sample testing data due to a problem associated with peak shape. However, your laboratory incident reports provide no evidence to support these conclusions. Both analysts also changed the clock prior to reanalyzing the samples.So what the heck is the point in injecting sample after sample into a HPLC within seconds of each other? I don't get it.
b. A QC analyst injected sample P140818008.lcd for the assay analysis of [redacted] (batch [redacted]) prior to the reported sample injections. The “trails” [sic] folder where the original sample injection file was saved had been deleted. Your response acknowledges that an analyst deleted eight injections, including the blank, six standards, and a sample.
c. A QC analyst deleted original test method validation data and admitted plans to fabricate sample preparation data. According to the HPLC audit trail, on October 7 and 8, the QC analyst injected two sets of similarly named samples of (b)(4) (#1:P141007001.lcd and #1:P 141007001.lcd) for an impurity analysis method validation study. Your analyst deleted data from the first set of injections and submitted only the second set in the validation documentation. The analyst stated that he planned to back-date the preparation data within the worksheets once all testing was complete. However, aside from balance scale tickets, your firm was unable to provide sample preparation data for either sample. Your response states that you abandoned the method validation study, but you continue to use that method for routine testing. In response to this letter, provide the method validation study that supports your current method for analyzing impurities in [redacted].
(Changing the clock - that's brilliant.)