Documentation sample analysis

Some types of Karl Fischer instruments provide special capability of moisture analysis by utilizing a ramping oven feature that can differentiate surface from bound moisture in a single analysis. Optimizing moisture methods is simplified by computer software available to fully document sample analysis data treatment. 

Figure 15.4 shows a procedure for the refilling of returnable containers with a chemical of assured quality. (This will require some combination of documentation, sampling and analysis to ensure that the chemical is of the correct type, and in the intended condition.) This is applicable to drums and plastic containers, and bottles, but some modifications are necessary for pressure systems, i.e. gas cylinders, covered by the Pressure Systems Safety Regulations 2000 including ... 

After the biological samples have been cleaned up, analytes are introduced to LC/MS for analysis. Approaches to shorten the sample analysis time are well documented. Two major strategies... 

Sampling Methods, Sample Analysis, and Area Survey Methodology, 32 Area Sampling and Survey Documentation, 33 Final Closure Survey Report and Closure Certification, 33 Postclosure Monitoring Requirements, 33... 

Different sampling techniques are documented for analysis of CCI4 in the air (Patnaik, P. 1997. Handbook of Environmental Analysis. Boca Raton, FL Lewis Publishers). 

Filters are required for dissolution sample collection. It is necessary to filter out the excipents that may cause interference in sample analysis. Appropriate recovery studies should be performed and documented. Any observed bias should be addressed. Filtration must be performed when the sample aliquots are withdrawn, not at a later time. 

Environmental samples may occasionally become legal evidence, and their possession must be traceable. An official document called the Chain-of-Custody Form serves the purpose of documenting sample transfer from one party to another. It is a record that tracks samples through their complete life span and serves as analysis request form. Over the years, the use of the COC became the industry standard regardless of whether the samples are being collected for legal purposes or not. 

Documenting sample transfer from one person to another is a critical legal issue, and many legal claims have been dismissed in court based on incomplete or incorrect COC forms. The sampling team must fill out the COC form with great care, not only because it may become a legal document but also because it is often the only written record related to sample identification, type, and requested analysis that the laboratory will get. 

The interpretation and implementation of published methods invariably differ at different laboratories due to diversity of utilized instruments, their incidental elements and supplies, and the differences in method interpretation. Each analytical method must be validated at the laboratory before it is used for sample analysis in order to demonstrate the laboratory s ability to consistently produce data of known accuracy and precision. Method validation includes the construction of a calibration curve that meets the acceptance criteria the determination of the method s accuracy and precision and the MDL study. A method SOPs must be prepared and approved for use. Method validation documentation is kept on file and should be always available to the client upon request. 

Prior to sample analysis, a test batch is required if (1) STD and QC pools need to be qualified, (2) there has been a significant lapse in time since any previous analysis, (3) the scientist does not have documentation with the assay or a similar assay. The test batch should contain minimally low, medium, and high QC at six replicates. Dilution QC samples may be included if dilutions are expected during sample analysis. The acceptance of PSAE is the same as described in intraassay precision and accuracy. 

The Contractor shall not proceed with the sample analysis until an acceptable initial calibration has been performed and documented according to the following criteria GC resolution, ion abundance ratios, retention times, and instrument sensitivity. 

The underlying principle of GLP requires that the retention of records, other documentation, samples and specimens should provide, wherever possible, the means for full study reconstruction. Thus, it follows logically that also samples from each batch of test and reference item should be collected and retained. In this way it can be ensured that any questions regarding the quality, purity, stability and identity of the test item, that might turn up during the Quality Assurance audit or the scientific assessment of the study, could be resolved by an independent analysis of the reserve sample, without necessitating the repetition of the study itself in case of major doubts about the test item. The requirement that a sample for analytical purposes from each batch of test item should be retained would therefore not seem to pose major problems of interpretation and implementation. 

In some instances, these recommended a priori acceptance criteria for model acceptance may be too restrictive and more lenient criteria may be appropriate with suitable justification and documentation. Model confirmation should precede the reporting of analytical results for validation samples. The standard curve for each in-study run (study sample analysis) should be monitored using the same criteria used during prestudy validation. 

During the prestudy evaluation phase, an attempt should be made to evaluate the variety of conditions that may reflect the execution and performance of the method during the in-study phase. The final conditions should be clearly documented in the analytical procedures prior to in-study sample analysis. As an example, robustness assessment could include incubation time tolerances, while ruggedness assessment could include changes in analysts and batch size (Table 4.7). Most robustness and ruggedness evaluations are empirical in nature however, more formal evaluations can also be used [29]. 

It is very likely that incomplete or missing records would prevent the verification of data integrity. Source records should be complete to facilitate an understanding of actual study conduct for critical phases of method development, method validation, and subject sample analysis. The records should confirm whether the testing was conducted in an appropriate manner, with well-designed and optimally controlled experiments. The documentation of actual laboratory events should demonstrate that the quantitative measures are suitable to achieve the objectives of the clinical or nonclinical protocol. The records should confirm that the reported results accurately reflect the actual concentration of the analyte in the biological matrix. It should be noted that the failure to adequately document critical details of study conduct has resulted in rejection of bioanalytical data for regulatory purposes. 

Although complete and contemporaneous documentation of study events is critical from a regulatory perspective, it should not be viewed solely as a regulatory requirement. It is also essential to the bioanalytical laboratory in its effort to demonstrate that a method is reliable and can produce high-quality data. Furthermore, comprehensive recording of study events can assist the bioanalytical laboratory in troubleshooting efforts, when unexpected problems occur during routine sample analysis. 

In cases where the study sponsor or pharmacokineticist5 assumes responsibility for selecting samples for repeat analysis, the bioanalytical laboratory should require and maintain written documentation of the request in the study file. The written documentation should identify the samples selected by the sponsor or pharmacokineticist, along with the basis for the selection. Ideally, the selection criteria used by the sponsor or pharmacokineticist should be provided to the bioanalytical laboratory in advance of sample analysis and maintained in the study file. Similarly, if the sponsor or pharmacokineticist assumes responsibility for determining the value reported for pharmacokinetic calculations, the SOP followed by the sponsor or pharmacokineticist in this regard should also be provided to the bioanalytical laboratory to facilitate a complete record for reconstructing the study conduct. 

The bottom line is that the lab maiiagement and analysts should use common sense in judging what quality assurance procedure should be implemented, based on the goal of the analysis, experience, available methods, time and cost constraints, and the like. But the closer you can adhere to accepted guidelines, the more confident you (and others) will be in your results. Remember, a proper analysis is more than simply receiving a sample and performing a one-shot analysis. If it is not properly documented, the analysis effort, time, and cost may be wasted. 

Other critical reagents are those that impact the sensitivity, ruggedness, and consistency of the assay and especially include the detection system. It is a recommendation that a list of critical reagents and criteria for their acceptance be identified before initiating sample analysis. These must also be sourced, characterized, documented, and stored under conditions defined by stability investigation. When in-house reagents make up any part of the immunoassay, it is important to define and document the source, preparation, expiration, storage conditions, and acceptance criteria for their use to ensure a reliable result. 

The established/validated format should be used during sample analysis. Changes to the format must be revalidated to the extent that a consistent format is confirmed. The acceptability of changes to critical reagents should be documented before placing them into the sample analysis assays. 

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