Development and validation of a method for the determination of sulfonamides in animal feed by modified QuEChERS and LC-MS/MS analysis

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• 作者：Renata Pereira Lopes^a ; ^{renatapl@ufmg.br} ; ^{renatapereiralopes@yahoo.com.br} ; É ; rica Eustá ; quia de Freitas Passos^b ; Juarez Fabiano de Alkimim Filho^b ; Eugê ; nia Azevedo Vargas^b ; Daniella Vasconcellos Augusti^b ; Rodinei Augusti^b ; ^{augusti@ufmg.br}
• 关键词：Animal feed ; Sulfonamides ; QuEChERS ; HPLC&ndash ; MS/MS
• 刊名：Food Control
• 出版年：2012
• 期刊代码：49_09567135
• 类别：abs
• 出版时间：November, 2012
• 卷：28
• 期：1
• 页码：192-198
• 文件大小：296 K

摘要

A multiresidue method for the quantification of 13 sulfonamides in animal feed is described. It involves the application of a modified QuEChERS procedure followed by HPLC-MS/MS (high performance liquid chromatography coupled to tandem mass spectrometry) analysis. The best conditions for the extraction solution and PSA (primary secondary amine) mass were determined. After optimization, the method was validated according to the European Commission Decision 2002/657/EC. The validation levels employed were 25, 50 and 75聽渭g聽kg^鈭?. Acceptable values were obtained for the following parameters: linearity (0.9864聽<聽r²聽<聽0.9993), decision limit (50.4聽渭g聽kg^鈭?聽<聽CC_伪聽<聽55.8聽渭g聽kg^鈭?), detection capability (50.7聽渭g聽kg^鈭?<CC_尾聽<聽55.8聽渭g聽kg^鈭?), limit of quantification (0.9聽渭g聽kg^鈭?聽<聽LOQ聽<聽7.1聽渭g聽kg^鈭?), accuracy (86.0聽<聽recovery rates聽<聽106.8), precision [(3.6聽<聽repeatability聽<聽19.5), (5.5聽<聽intermediate precision聽<聽21.6)], measurement uncertainty (MU) (4.1聽<聽MU聽<聽32.6) and selectivity. These findings met the Codex requirements, which allow for the routine use of the method by the laboratories linked to the Ministry of Agriculture, Livestock and Food Supply of Brazil. Finally, the method was applied to real samples and only one of them showed positive for sulfamethazine, however, with a concentration below the LOQ of the method.