Abstract
A rapid HILIC-MS method was developed for measuring the genotoxic impurities aziridine and 2-chloroethylamine. Sample preparation was simple and direct without requiring derivatization. Paired with a 1.5 min isocratic UHPLC separation, sample analysis could be completed in less than 5 min. Linearity was established from 0.5 μg/L to 10 μg/L for both target analytes. For main components at 100 g/L, this equates to 5 parts per billion (ppb) detectability using a benchtop, single quadrupole detector. Three model matrices were evaluated (glycine, phenylalanine, and the pharmaceutical drug asunaprevir), and the method was able to provide suitable repeatability (<10% RSD) and accuracy (±10%) at 5 μg/L concentrations.•Direct sample preparation without derivatization as is needed for GC analyses•Less than 5 min required for sample preparation and HILIC-MS analysis•Part per billion sensitivity in multiple test matrices with good recovery
Highlights
ABSTRACTA rapid HILIC-MS method was developed for measuring the genotoxic impurities aziridine and 2-chloroethylamine
The required analytical sensitivity for assessing these components in pharmaceutical intermediates, active substances, or products will be dictated by the dosage amount and duration, typically low parts per million limits of detection (LOD) are needed
Douša et al described a method using hydrophilic interaction liquid chromatography coupled with mass spectrometry detection (HILIC–MS) for measuring 2-chloro-N-(2-chloroethyl) ethanamine in vortioxetine using an HPLC mixed mode column (Primesep B, SIELC Technologies), making it unclear if the dominant retention mechanism was HILIC partitioning or ion exchange [9]
Summary
Direct, and sensitive determination of aziridine and 2-chloroethylamine by hydrophilic interaction liquid chromatography-mass spectrometry. ABSTRACTA rapid HILIC-MS method was developed for measuring the genotoxic impurities aziridine and 2-chloroethylamine. Sample preparation was simple and direct without requiring derivatization. UHPLC separation, sample analysis could be completed in less than 5 min. For main components at 100 g/L, this equates to 5 parts per billion (ppb) detectability using a benchtop, single quadrupole detector. Direct sample preparation without derivatization as is needed for GC analyses Less than 5 min required for sample preparation and HILIC-MS analysis Part per billion sensitivity in multiple test matrices with good recovery. Subject Area: More specific subject area: Method name: Name and reference of original method: Resource availability: Chemistry Analytical Chemistry HILIC-MS detection of aziridine and 2-chloroethylamine N/A All resources commonly available
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