Development of an ASE‐GC‐MS/MS method for detecting dinitolmide and its metabolite 3‐ANOT in eggs. (15th August 2018)

• Record Type: Journal Article
• Authors: Zhao, Xia; Wang, Bo; Xie, Kaizhou; Liu, Yanan; Zhang, Yangyang; Wang, Yajuan; Liu, Chujun; Guo, Yawen; Bu, Xiaona; Zhang, Genxi; Zhang, Tao; Dai, Guojun
• Is Part Of: Journal of mass spectrometry. Volume 53:Number 10(2018)
• Page Start: 976
• Page End: 985
• Publication Date: 2018-08-15
• Subjects: 3‐ANOT -- ASE -- dinitolmide -- egg -- GC‐MS/MS; Mass spectrometry -- Periodicals; 543.65
• DOI: 10.1002/jms.4267
• Languages: English
• ISSNs: 1076-5174

Abstract

Abstract: An accelerated solvent extraction coupled with gas chromatography‐tandem mass spectrometry (ASE‐GC‐MS/MS) method for detecting dinitolmide residue and its metabolite (3‐amino‐2‐methyl‐5‐nitrobenzamide, 3‐ANOT) in eggs was developed and optimized. The samples were extracted using ASE with acetonitrile as the extractant and were purified by passage through a neutral alumina solid‐phase extraction column. Then, the samples were analyzed using the GC‐MS/MS method. The optimized method parameters were validated according to the requirements set forth by the European Union and the Food and Drug Administration. The average recoveries of dinitolmide and 3‐ANOT from eggs (egg white, egg yolk, and whole egg) at the limit of quantification (LOQ), 0.5 maximum residue limit (MRL), 1 MRL, and 2 MRL were 82.74% to 87.49%, the relative standard deviations (RSDs) were less than 4.63%, and the intra‐day RSDs and the inter‐day RSDs were 2.96% to 5.21% and 3.94% to 6.34%, respectively. The limits of detection and the LOQ were 0.8 to 2.8 μg/kg and 3.0 to 10.0 μg/kg, respectively. The decision limits (CCα ) were 3001.69 to 3006.48 μg/kg, and the detection capabilities (CCβ ) were 3001.74 to 3005.22 μg/kg. Finally, the new method was successfully applied to the quantitative determination of dinitolmide and 3‐ANOT in 50 commercial eggs from local supermarkets.