Sensitive quantitation of residual phenylhydrazine in antipyrine by LC-ICP-MS with iodo derivatization.

Phenylhydrazine is a genotoxic impurity commonly used as a raw material in active pharmaceutical ingredients. In this study, a novel method, using inductively coupled plasma-mass spectrometry combined with two-dimensional liquid chromatography (LC-ICP-MS), was employed for the quantitation of residual phenylhydrazine in antipyrine. The compound 2,3,5-triiodobenzoyl chloride, which contains three iodine atoms, was investigated as a derivatization reagent.

Development and validation of a sensitive GC-MS method for the determination of alkylating agent, 4-chloro-1-butanol, in active pharmaceutical ingredients.

The analysis of genotoxic impurities (GTIs) in active pharmaceutical ingredients (APIs) is a challenging task. The target detection limit (DL) in an API is typically around 1 ppm (1 µg/g API). Therefore, a sensitive and selective analytical method is required for their analysis.

Novel sensitive determination method for a genotoxic alkylating agent, 4-chloro-1-butanol, in active pharmaceutical ingredients by LC-ICP-MS employing iodo derivatization.

An alkylating agent, 4-chloro-1-butanol, is a genotoxic impurity (GTI); it may be generated during the synthesis of active pharmaceutical ingredients (APIs). For the trace-level detection of GTIs in APIs, usually, gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-mass spectrometry (LC-MS) is employed. In this study, a novel LC-inductively coupled plasma (ICP)-MS method was developed and validated.

Determination of aluminum in large volume parenteral drug products used in total parenteral nutrition therapy by ICP-MS with a dynamic reaction cell.

The proposed method was developed for the determination of aluminum (Al) in large volume parenteral (LVP) drug products used in total parenteral nutrition (TPN) therapy. The determination of Al in LVP drug products was performed by an inductively coupled plasma mass spectrometer equipped with a dynamic reaction cell (DRC-ICP-MS). DRC-ICP-MS conditions for the analysis of Al were studied to obtain the best signal to background (S/N) ratios.