Drug product analysis, sample

For high reproducibility of migration times and peak areas the sample matrix should be identical for all samples analyzed together. While this is challenging for forensic applications where analytes in whole blood or urine are determined, this requirement can be fulfilled easily in pharmaceutical analysis. After sample preparation of the drug product, the sample matrix is similar in most cases. The composition of blood or urine depends on its source. Thus, the changing sample matrix has more impact on the quality of the CE analysis. 

Sample Preparation Perspectives in Drug Product Analysis... 

The recovery of a sample preparation must be assessed, because the recovery determines the accuracy of the analysis. For drug substance and drug product analysis, recovery of 100% is generally required to maintain required levels of accuracy and precision. For biological samples, less than quantitative recovery is generally acceptable if the recovery is reproducible. 

Evaluating through factory inspections, including the collection and analysis of associated samples, the conditions and practices under which drugs and drug products are manufactured, packed, tested, and held, and... 

SAMPLE PREPARATION FOR HPLC ANALYSIS OF DRUG PRODUCTS... 

Accuracy. Sample solutions of known concentration (e.g., spiked placebo) are used for the accuracy determination. Experimental work may be organized so that the same stock solutions are used to prepare both linearity and accuracy solutions. The accuracy solution must be exposed to normal test conditions (e.g., mixing in a heated dissolution vessel). Determine any bias that is caused by the sampling and analysis of the solutions. If a dissolution profile of the drug product is required, accuracy determinations at different concentrations of the required profile will need to be performed (e.g., at 40, 75, and 110% of theoretical release). The results are reported as percent theory. 

Robustness of the sample analysis scheme Three samples will be prepared by spiking product B (known to contain < 0.05 ppm of element A) with element A to 0.5 ppm of element A in the drug product. 

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