Pharmaceutical manufacture sampling time

Identifying pharmaceuticals, whether APIs or excipients used to manufacture products, and the end products themselves is among the routine tests needed to control pharmaceutical manufacturing processes. Pharmacopoeias have compiled a wide range of analytical methods for the identification of pharmaceutical APIs and usually several tests for a product are recommended. The process can be labor-intensive and time-consuming with these conventional methods. This has raised the need for alternative, faster methods also ensuring reliable identification. Of the four spectroscopic techniques reviewed in this book, IR and Raman spectroscopy are suitable for the unequivocal identification of pharmaceuticals as their spectra are compound-specific no two compounds other than pairs of enantiomers or oligomers possess the same IR spectrum. However, IR spectrometry is confronted with some practical constraints such as the need to pretreat the sample. The introduction of substantial instrumental improvements and the spread of attenuated total reflectance (ATR) and IR microscopy techniques have considerably expanded the scope of IR spectroscopy in the pharmaceutical field. Raman spectroscopy,... 

It has been proved in several research papers that water is the most important factor in the component s degradation of ORSs. To proceed with the study, the pharmaceutical formulation was prepared by a pharmaceutical manufacture. The batch was packed in six types of packaging material. After storage of samples for 36 weeks maintained at ambient temperature, at ambient temperature and 76% relative humidity, and at 40°C with 80% relative humidity, analyses of water determination were made at different intervals of time. Water determination was performed by loss on drying at 50°C and Karl Fisher methods. 

We expect that the focus of pharmaceutical QC/QA will be broadened in the near future. Traditionally we have concentrated on the quality of products at the time manufacture is complete, with stability being very largely evaluated from retained stability samples. It is probable that more attention will be given to monitoring the quality of products in the channels of distribution and even, in some instances, under conditions... 

HPLC precision is critical in pharmaceutical analysis.For most pharmaceutical assays under a good manufacturing practice (GMP) environment, retention time and peak area precision of <2.0% RSD must be demonstrated before any samples can be analyzed. This section reviews the fundamental principles of HPLC precision and offers practical guidelines for its enhancement. The reader is referred to Reference 18 for a more detailed treatment of this topic. 

Interestingly, the two methods published for quantification of sunitinib used either HPLC [114] or UPLC [113] but the analytical time periods were of similar duration (run time of 3 min and 4 min, respectively). Of note, we observed during the course of our own method development [122] the presence of two peaks with the same molecular mass/signal transition for sunitinib, which, to the best of our knowledge, has not been reported elsewhere [113, 114, 123], The phenomenon was known, however, and is due to a Z-E isomerization reaction of sunitinib [124], Previous studies by the sunitinib manufacturer have shown that E isomer can be generated from the Z isomer in a reversible manner in solution [124], The rate of interconversion between the Z-E configurations in solution is dependent on a number of factors, most notably exposure to light. In our studies [122], we found that both isomers could be detected in the pharmaceutical preparation (tablet) at ratios of about 1 2, as well as in patients plasma samples (variable ratios). 

The elution method involves scraping off the separated zones of samples and standards and elution of the substances from the layer material with a strong, volatile solvent. The eluates are concentrated and analyzed by use of a sensitive spectrometric method, gas or liquid column chromatography, or electroanalysis. Scraping and elution must be performed manually because the only commercial automatic micropreparative elution instrument has been discontinued by its manufacturer. The elution method is tedious and time-consuming and prone to errors caused by the incorrect choice of the sizes of the areas to scrape, incomplete collection of sorbent, and incomplete or inconsistent elution recovery of the analyte from the sorbent. However, the elution method is being rather widely used (e.g., some assay methods for pharmaceuticals and drugs in the USP Pharmacopoeia). 

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