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Analysis of sulfonylurea herbicides by gas–liquid chromatography III—mass spectrometry and multiresidue determination
Author(s) -
Klaffenbach Peter,
Holland Patrick T.
Publication year - 1993
Publication title -
biological mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 1052-9306
DOI - 10.1002/bms.1200221003
Subject(s) - chemistry , diazomethane , electron ionization , sulfonylurea , mass spectrometry , derivatization , chromatography , gas chromatography , gas chromatography–mass spectrometry , chemical ionization , mass spectrum , ion , ionization , organic chemistry , medicine , insulin , endocrinology
A method is described for the determination of sulfonylurea herbicides by gas chromatography (GC). Chlorimuronethyl, cinosulfuron, primisulfuron‐methyl, thifensulfuron‐methyl, triasulfuron and tribenuron‐methyl were converted into thermostable derivatives by reaction with diazomethane in ethyl acetate. The resulting N , N ′‐dimethyl derivatives were suitable for analysis by GC. Two of the herbicides formed multiple derivatives. The identity of the derivatives was confirmed using chemical ionization and electron impact mass spectrometry and nuclear magnetic resonance. The proposed structures of the ions in the electron impact mass spectra were confirmed using high‐resolution, metastable ion decomposition and deuterium‐labelling techniques. The derivatization was incorporated into multimethods for the residue analysis of the six sulfonylurea herbicides in water, soil and wheat samples. Recoveries ranged from 88% to 122% in water (0.1 μg 1 −1 ), 53% to 99% in soil (1 μg kg −1 ) and 41% to 120% in wheat (0.2 mg kg −1 ).