期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 395, 期 2, 页码 465-471出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-009-2962-y
关键词
Amitrole; Precolumn derivatization; 4-Chloro-3,5-dinitrobenzotrifluoride (CNBF); High-performance liquid chromatography; Apple
资金
- Major State Basic Research Development Program of China [2007CB109105]
- National High Technology Research and Development Program of China [2006AA10A203]
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-chloro3,5-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 degrees 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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