Supporting documentation, sample analysis

After completing the necessary preparation procedures, the Sample Preparation Section personnel place extracts in sealed, labelled vials and store them in specially designated refrigerators at 2-6°C. Organic extracts will stay refrigerated until the time of analysis. Metal digestates are stored at room temperature. Completed preparation bench sheets and other support documentation become part of the permanent sample record. When we request that samples be composited at the laboratory, for most types of analysis the compositing will be typically done at the Sample Preparation Section. 

Each data package represents a group of samples usually delivered to the laboratory under one COC Form. All of the requested analyses are combined in one data package, and each analysis has its own laboratory QC checks and support documentation. (Occasionally, laboratories may combine several small groups of samples with separate COC Forms into one data package, usually if the same batch QC checks apply to all groups.)... 

In forensic cases it is important to ensure that all samples are labelled correctly and that there is a chain of custody (see Section 5.3) back to the point from where the sample was taken. Consider the case of two athletes who have urine samples taken for analysis for the presence of illegal drugs. One of the tests is positive and the other negative. The analyst who gives evidence in court must be certain beyond reasonable doubt that the positive result from the urine sample can be connected to the eorrect athlete. This can be achieved if the samples and supporting documentation are clearly and accurately labelled. 

The previous sections in this chapter addressed the process of validating the method and documenting the results in a final validation report. When reviewing the analytical data for the study samples the validation report and associated tables and supporting documentation must be carefully reviewed for accuracy and scientific content, to ensure that the necessary experiments have been run and that the data supports the original uncertainty tolerances (Section 9.3). In addition to the validation report, the final method must be reviewed and approved for sample analysis. Specific acceptance criteria that will be used during sample analysis should be documented in the approved method or equivalent SOP. 

QA requires the efficient analysis of many samples to support routine production release and stability programs. Methods are typically established in the analytical development group. Efficiency and convenience issues, including the speed of media preparation and the relative convenience of data handling and documentation, are important here. While compliance is important in all aspects of the pharmaceutical industry, QA functions must approach compliance perfection. Depending upon the facility, the automated apparatus may be tailored to specific methods with fixed configurations. Dissolution methods may be routine enough that a custom system, optimized for productivity, may be justified. Compliance of USP and use of industry standard apparatus is important to maintain compatibility with other company laboratories or in the case contract laboratory services are required. 

A typical instrument for XRD of a working catalyst consists of a (commercial) powder diffraction instrument, a reaction cell, and the auxiliary equipment for reactant dosing and product analysis. It is desirable to use a computer system that simultaneously controls all these functions or at least records the sample temperature and experiment time together with the diffraction information. A single experiment characterizing a catalyst under working conditions typically produces a large amount of data, the analysis of which consumes much more time than the experiment. Thus, accurate documentation is mandatory and is best supported by automatic routines. 

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