Abstract
A novel method based on solid-phase extraction was studied for the extraction of amitrole (3-amino-1,2,4-triazole), and its residue determination in apples has been developed. The samples were derivatized with 4-chloro-3,5-dinitrobenzotrifluoride (CNBF). The derivatization conditions and the influence of elution composition on the separation were investigated. In pH 9.5 H3BO3–Na2B4O7 media, the reaction of amitrole with CNBF was complete at 60°C after 30 min. The separation of derivatized amitrole was achieved at room temperature within 13 min by gradient elution mode with cetyltrimethylammonium bromide in mobile phase as ion-pair reagent. The method correlation coefficient was 0.9996, in concentrations ranging from 1.66 to 415 mg L−1. The calculated recoveries of the proposed method were from 94.17% to 105.67%, and relative standard deviations were 1.57% to 6.44% in the application to the quantitative determination of amitrole in apples. The detection limit of amitrole was 0.10 mg L−1 with a signal-to-noise ratio of 3.
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Acknowledgment
This work was supported by the Major State Basic Research Development Program of China (973 program, no. 2007CB109105) and the National High Technology Research and Development Program of China (863 Program, no. 2006AA10A203).
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Sun, Y., Luo, L., Wang, F. et al. Ion-pairing high-performance liquid chromatography determination of amitrole in apple after solid-phase extraction and precolumn derivatization. Anal Bioanal Chem 395, 465–471 (2009). https://doi.org/10.1007/s00216-009-2962-y
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DOI: https://doi.org/10.1007/s00216-009-2962-y