Determination and confirmation of nitrofuran residues in honey using LC-MS/MS

被引:56
作者
Lopez, Mayda I.
Feldlaufer, Mark F.
Williams, Anthony D.
Chu, Pak-Sin
机构
[1] USDA, Ctr Vet Med, Laurel, MD 20708 USA
[2] USDA, Bee Res Lab, Beltsville, MD 20705 USA
[3] USDA, Off Regulatory Affairs, Atlanta, GA 30309 USA
关键词
nitrofurans; honey; LC-MS/MS; method;
D O I
10.1021/jf0625712
中图分类号
S [农业科学];
学科分类号
09 ;
摘要
A method was developed for the determination and confirmation of furazolidone, nitrofurazone, furaltadone, and nitrofurantoin as their side-chain residues in honey using liquid chromatography-tandem mass spectrometry (LC-MS/MS). An initial solid-phase extraction cleanup of the honey samples was followed by overnight hydrolysis and derivatization of the nitrofuran side-chain residues with 2-nitrobenzaldehyde. After pH adjustment and liquid-liquid extraction, the extracts were assayed by LC-MS/MS using electrospray ionization in the positive ion mode. The method was validated at concentrations ranging from 0.5 to 2.0 ppb with accuracies of 92-103% and coefficients of variation of <= 10%. The lowest calibration standard used (0.25 ppb) was defined as the limit of quantitation for all four nitrofuran side-chain residues. The extracts and standards were also used for confirmatory purposes. Honey from dosed beehives was assayed to study the stability of the nitrofuran residues and to demonstrate the effectiveness of the method.
引用
收藏
页码:1103 / 1108
页数:6
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