Impurities formulation-related

An MEKC method for the determination of ibuprofen, codeine phosphate hemihydrate, their nine potential degradation products, and impurities in a commercial tablet formulation was developed, optimized, and fully validated according to ICH guidelines and submitted to the regulatory authorities. The optimized system containing ACN as organic modifier allowed baseline separation of ibuprofen, codeine, and nine related substances within 12 min. 

Source Componnds detected in major formulations and products are included, e.g., benzene detected in air, water, or soil samples may be related or have originated from various types of petroleum spills such as gasoline or diesel fuel. In some instances, the compound of concern may be an impurity in the material released to the enviromnent or it may be naturally present in various types of vegetation. 

The reason for this is that if a stable, optically transparent emulsion is to be obtained, the relationship between the amount of the oil phase and the surfactants has to be within a relatively narrow range. Microemulsion elec-trokinetic chromatography has been shown to be a highly applicable technique for the analysis of complex mixtures such as multicomponent formulations and drug-related impurities. This technique opens a new way to determine water-insoluble neutral species such as steroids, which are difficult to analyze by CE. It is therefore likely that the MEEKC method will be increasingly applied for pharmaceutical and biopharmaceutical analyses in coming years. 

Analytical Development of API and Drug Products. Early methods to support synthetic and formulation developments are often developed in the form of potency assay, impurities/related substance assay, dissolution, Karl Fischer, identity, chiral method, and content uniformity. These analytical methods are developed and validated in a fast and timely manner to support all phase II studies. 

In order to identify any excipient- and packaging-related impurities in the formulation, placebo cores and hlm-coated placebos, were prepared using the same excipients as in the active tablets. The placebo cores and film-coated placebos, as well as active cores and hlm-coated active tablets were set up on a stability study in high density polyethylene (HDPE) bottles with and without desiccant and in foil-foil blisters. At the designated time intervals, the tablets were tested for purity by gradient HPLC analysis. 

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