期刊
ANALYTICA CHIMICA ACTA
卷 635, 期 2, 页码 222-226出版社
ELSEVIER
DOI: 10.1016/j.aca.2009.01.022
关键词
Glyphosate; Pre-column derivatization; 4-Chloro-3,5-dinitrobenzotrifluoride; High-performance liquid chromatography
资金
- Major State Basic Research Development Program of China [2007CB109105]
- National High Technology Research and Development Program of China [2006AA10A203]
A pre-column derivatization high-performance liquid chromatographic method for glyphosate analysis has been developed. Derivatization of glyphosate was performed with 4-chloro-3,5-dinitrobenzotrifluoride (CNBF). In pH 9.5 H3BO3-Na2B4O7 media, the reaction of glyphosate with CNBF completed at 60 degrees C for 30 min. The labeled glyphosate was separated on a Kromasil C18 column (250 mm x 4.6 mm, 5 mu m) at room temperature and UV detection was applied at 360 nm. The separation of labeled glyphosate was achieved within 15 min by gradient elution mode. Compared to other pre-column derivatization. this derivatization was performed more mildly, the derivative was more stable, and the detection limits of a few reagents were higher than CNBF, except 9-fluorenylmethyl chloroformate (FMOC-Cl) using fluorescence and mass spectrometry, however, this reagent avoid to be removed after derivatization like FMOC-Cl. The detection limit of glyphosate was 0.009 mg L-1 (S/N = 3) without preconcentration and reach MRL, which is set at the level of 0.1 mg L-1 in China. The method linearity correlation coefficient was 0.9999, in concentrations ranging from 0.3 to 48.5 mg L-1. The proposed method has been applied to the quantitative determination of glyphosate in environmental water with recoveries of 91.80-100.20% and R.S.D. of 2.27-6.80, depending on the sample investigated. (C) 2009 Elsevier B.V. All rights reserved.
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