Effect of pressure on secondary structure of proteins under ultra high pressure liquid chromatographic conditions.

There are several spectroscopic techniques such as IR and CD, that allow for analyzing protein secondary structure in solution. However, a majority of these techniques require using purified protein, concentrated enough in the solution, to produce a relevant spectrum. Fundamental principles for the usage of reversed-phase ultra high pressure liquid chromatography (UHPLC) as an alternative technique to study protein secondary structures in solution were investigated.

Investigation of Metformin HCl lot-to-lot variation on flowability differences exhibited during drug product processing.

The purpose of this study was to determine the cause for flowability difference observed during drug product processing when different Metformin HCl drug substance batches of varying age were used. It was found that the lead time (age) between the final step (milling) in the manufacturing process of the Metformin HCl drug substance could be a factor. The lead time had an impact on flowability of Metformin/excipient blends during drug product processing even though these batches had no apparent differences in their release specifications.

Combined application of high resolution and tandem mass spectrometers to characterize methionine oxidation in a parathyroid hormone formulation.

Identification and monitoring of degradation products is a critical aspect of drug product stability programs. This process can present unique challenges when working with complex biopharmaceutical formulations that do not readily lend themselves to straightforward HPLC analysis. The therapeutic 34 amino acid parathyroid hormone fragment (PTH1-34) contains methionine (Met) residues at positions 8 and 18.

Evaluation of transmission and reflection modalities for measuring content uniformity of pharmaceutical tablets with near-infrared spectroscopy.

This paper examines how one may assess spectral changes with instrument configuration (or composition), in combination with the spectral changes in the measurement that are caused by experimental effects, and subsequently select an appropriate measurement modality for tablet content uniformity determination with near-infrared (NIR) spectroscopy. Two NIR spectrometers furnished with three configurations in the sample measurement interface were evaluated. One spectrometer, Bruker MPA (multiple purpose analyzer), was equipped with two measurement modalities, diffuse transmission (DT) and diffuse reflection based on integrating sphere optics (DR/IS).

Characterization of moisture-sensitive raw materials with simple spectroscopic techniques.

The quality of raw materials used in a synthetic process needs to be properly controlled in order to ensure optimal reaction conversion and desired quality of the resulting product. For air and water sensitive raw materials, quantitative analysis can be a challenging task. Spectroscopic techniques possess advantages of simple operation, fast analysis, low consumable costs and high sample throughput for the analysis of reactive raw materials.