Ion-pairing high-performance liquid chromatography determination of amitrole in apple after solid-phase extraction and precolumn derivatization.
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 H(3)BO(3)-Na(2)B(4)O(7) 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.
Sun
Yan
Y
College of Agriculture and Biotechnology, China Agricultural University, No. 2 Yuanmingyuan West Road, Beijing, 100193, China.
Luo
Laixin
L
Wang
Fang
F
Li
Jianqiang
J
Cao
Yongsong
Y
D000640:Amitrole / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005464:Fluorobenzenes; D006540:Herbicides / Q000032:analysis*; D027845:Malus / Q000737:chemistry*; D009574:Nitro Compounds; D012680:Sensitivity and Specificity; D052616:Solid Phase Extraction / Q000379:methods*
D005464:Fluorobenzenes; D006540:Herbicides; D009574:Nitro Compounds; C539305:4-chloro-3,5-dinitrobenzotrifluoride; D000640:Amitrole