Quantitative method for determination of 3,3‐dimethylallyl bromide genotoxic impurity in Tazarotene drug substance by GC‐MS

Abstract

A highly sensitive gas chromatography‐mass spectrometry quantitative method was developed for 3,3‐dimethylallyl bromide genotoxic impurity in the tazarotene drug substance. The method was validated by following the International conference for harmonization Q2 (R1) guideline for the limit test of 3,3‐dimethylallyl bromide genotoxic impurity in the tazarotene drug substance. The 148 m/z, 150 m/z, and 69 m/z ions were selected to get a response in mass spectrometry for 3,3‐dimethylallyl bromide. DB‐1 (30 mm × 0.25 × 1.0 µm) column was used for the separation of 3,3‐dimethylallyl bromide from the sample matrix. The limit of detection and limit of quantitation for 3,3‐dimethylallyl bromide in this method was 0.7 and 2.1 ppm, respectively. The method was precise and accurate at limit of quantitation level, 1.7% RSD was observed at limit of quantitation precision and 100.9% recovery observed at limit of quantitation accuracy, it was linear from the 5 to 20 µg/L, the correlation coefficient (r) was 0.9996.

An orthogonal approach for method development and validation of three potential halo alkyl alcohol genotoxic impurities in miglitol drug substance by fast gas chromatography–mass spectrometry

“…Analytical methods are available for assay and related substance determination of miglitol [10][11][12][13][14][15][16][17][18][19]. Many researchers had performed quantitative determination of genotoxic impurities in different drug substances by using HPLC, UPLC, GC, IC, GC-MS, and LC-MS techniques [20][21][22][23][24][25][26][27][28]. As per the authors' knowledge, this is the first analytical GC-MS method for simultaneous determination of 2-chloro ethanol, 2-bromo ethanol, and 2-iodo ethanol without derivatization.…”