期刊
ANALYTICA CHIMICA ACTA
卷 1039, 期 -, 页码 59-64出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2018.08.041
关键词
FT-ICR-MS; Fraction collector; Organic impurities; Accurate mass; Isotopic fine structures
A strategy to determine the elemental composition of organic impurities in commercial preparations was established by combining high-performance liquid chromatography (HPLC)-Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) and fraction collector with direct infusion-FT-ICR-MS (DI-FT-ICR-MS). Under HPLC-FT-ICR-MS mode, all impurities in model sample were chromatographically separated and collected by fraction collector according to their retention time. The accurate mass of each impurity and their candidate formulae under 1 ppm mass tolerance were calculated. Subsequently, theoretical isotopic fine structures (IFSs) of the candidate formulae were generated. Furthermore, the collected fractions were tested and the experimental IFSs of impurities were acquired by DI-FT-ICR-MS mode. Finally, the elemental composition of all impurities was decisively determined by comparing the experimental and theoretical IFSs. Our results demonstrate that the combined strategy is effective in separating impurities and acquiring accurate mass by HPLC-FT-ICR-MS, obtaining the appropriate samples by fraction collection technology for DI-FT-ICR-MS, and acquiring the IFSs of impurities by DI-FT-ICR-MS. It could be concluded that the strategy is an accurate and standard independent approach to determine the elemental composition of organic impurities in commercial preparations. (C) 2018 Elsevier B.V. All rights reserved.
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