Degradation and Impurity Analysis for Pharmaceutical Drug Candidates

Quantitative 1H NMR. Development and Potential of an Analytical Method: An Update

“…For example, this can be due to formation of a chemical equilibrium depending on the solvent or storage conditions in general. 160 In summary, static RC is relatively easy to address, and may be reduced by additional purification (if practical). This often is due to chemicals that stem from the isolation procedure such as residual solvents, stationary phases, and co-crystallizing compounds.…”

“…These two reports, as well as the studies mentioned below, demonstrate the potential of qHNMR as a validation tool for the characterization of bioactive NPs. 3 A review on forced degradation studies for pharmaceutical drug candidates and the identification and quantitation of degradation products with qHNMR was published by Alsante et al 160 A report by Mohn et al described the purity evaluation of glucosinolates (e.g., 9) isolated from Isatis tinctoria with qHNMR. 68 A publication on Angelica sinensis used a combination of 1D-and 2D-NMR methods to determine the absolute amounts of 41 and six of its derivatives, in addition to establishing relative quantitative relationships within a series of phenylpropanoids, falcarindiol (42) polyacetylene derivatives, and unsaturated fatty acids present in a bioactive fraction of hydroalcoholic Angelica preparation.…”

“…Static RC is found when the kind and level of impurities present in a sample remain constant over time, while dynamic complexity describes the cases where impurity levels change over time and/or the composition of impurities change. For example, this can be due to formation of a chemical equilibrium depending on the solvent or storage conditions in general . In summary, static RC is relatively easy to address and may be reduced by additional purification (if practical).…”

Mass spectrometry-based structure elucidation of small molecule impurities and degradation products in pharmaceutical development

“…Given the starting molecule (e.g. drug API) and transformations, potential impurity structures can be deduced with software for organic reactivity prediction [86][87][88][89]. However, this approach does not guarantee that all masses are annotated since some impurities (e.g.…”

Supercritical Fluid Chromatography of Drugs: Parallel Factor Analysis for Column Testing in a Wide Range of Operational Conditions

“…In addition, this technique is considered as green due to its low consumption of organic solvents [2] that are toxic, expensive, and harmful to environment [3]. Therefore, SFC recently showed great success in many fields, such as the separation and detection of PAHs and petroleum related compounds [4–7], oligomers and polymers [8], food residues [9], unpermitted addition and misuse of dyes in different foodstuffs [10], cosmetics and body care products [11], pharmaceutical separation [12], drug development and discovery [3, 13–15], impurity profiling [16–18], and drug testing [1, 19, 20]. …”