Volume 12 Issue 4
Sep.  2022
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Yanfang Zhao, Jingkun Li, Hanyi Xie, Huijuan Li, Xiangfeng Chen. Covalent organic nanospheres as a fiber coating for solid-phase microextraction of genotoxic impurities followed by analysis using GC-MS[J]. Journal of Pharmaceutical Analysis, 2022, 12(4): 583-589. doi: 10.1016/j.jpha.2021.12.002
Citation: Yanfang Zhao, Jingkun Li, Hanyi Xie, Huijuan Li, Xiangfeng Chen. Covalent organic nanospheres as a fiber coating for solid-phase microextraction of genotoxic impurities followed by analysis using GC-MS[J]. Journal of Pharmaceutical Analysis, 2022, 12(4): 583-589. doi: 10.1016/j.jpha.2021.12.002

Covalent organic nanospheres as a fiber coating for solid-phase microextraction of genotoxic impurities followed by analysis using GC-MS

doi: 10.1016/j.jpha.2021.12.002
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This work was supported by the Key Research and Development Program of Shandong Province (Grant No.: 2019GSF111001), the National Natural Science Foundation of China (Grant No.: 21906096), the Youth Science Funds of the Shandong Academy of Sciences (Grant No.: 2019QN009), the Youth Ph.D. Cooperation Funds of Qilu University of Technology (Shandong Academy of Sciences, Grant No.: 2018BSHZ0029), and the Program for Taishan Scholars of Shandong Province (Grant No.: tsqn202103099).

  • Received Date: Mar. 09, 2021
  • Accepted Date: Dec. 05, 2021
  • Rev Recd Date: Dec. 04, 2021
  • Publish Date: Dec. 08, 2021
  • Covalent organic nanospheres (CONs) were explored as a fiber coating for solid-phase microextraction of genotoxic impurities (GTIs) from active ingredients (AIs). CONs were synthesized by an easy solution-phase procedure at 25℃. The obtained nanospheres exhibited a high specific surface area, good thermostability, high acid and alkali resistance, and favorable crystallinity and porosity. Two types of GTIs, alkyl halides (1-iodooctane, 1-chlorobenzene, 1-bromododecane, 1,2-dichlorobenzene, 1-bromooctane, 1-chlorohexane, and 1,8-dibromooctane) and sulfonate esters (methyl p-toluenesulfonate and ethyl p-toluenesulfonate), were chosen as target molecules for assessing the performance of the coating. The prepared coating achieved high enhancement factors (5097-9799) for the selected GTIs. The strong affinity between CONs and GTIs was tentatively attributed to π-π and hydrophobicity interactions, large surface area of the CONs, and size-matching of the materials. Combined with gas chromatography-mass spectrometry (GC-MS), the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range (0.2-200 ng/g) with a low detection limit (0.04-2.0 ng/g), satisfactory recovery (80.03%-109.5%), and high repeatability (6.20%-14.8%) and reproducibility (6.20%-14.1%). Therefore, the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.
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