3,5-Dinitrosalicylic acid hydrazide (DNSAH) is the metabolite of the antibacterial nitrofuran nifursol. A simple and accurate analytical method to determine 3,5-Dinitrosalicylic acid hydrazide in honey by solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) has been established. The honey sample was hydrolyzed under acidic conditions and derivatized with 2-nitrobenzaldehyde in the dark for 16 h followed by solid-phase extraction and column chromatography. Detection was performed using an electrospray ionization source (ESI - ) and multiple reaction monitoring (MRM) mode, and quantified by internal standard method. It was shown that the detection limit (LOD) and quantitative limit (LOQ) of DNSAH in honey were 0.1 and 0.3 μg/kg, respectively. Good linear relationships between peak areas and mass concentrations of the analyte were achieved in the range of 0.1~200 μg/L, with the correlation coefficient (r) greater than 0.9991. Under the concentration levels of 0.2, 0.5, 1.0, 2.0μg/kg, the average recovery rate were between 98.5 ~ 102.3% and the relative standard deviation (RSD) were between 1.1 ~ 5.4%. The results indicate that the method is simple, rapid, sensitive and reproducible, which can be used for determination of DNSAH in different types of honey.
Determination of 3,5-Dinitrosalicylic Acid Hydrazide in Honey by Solid-phase Extraction-ultra Performance Liquid Chromatography-tandem Mass Spectrometry
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rui chen, Jiaxuan Li, Zhiwei Yang, Xiang Li, Fengmei Zhu, Jun Li, Jinjie Zhang; Determination of 3,5-Dinitrosalicylic Acid Hydrazide in Honey by Solid-phase Extraction-ultra Performance Liquid Chromatography-tandem Mass Spectrometry. J Food Prot doi: https://doi.org/10.4315/JFP-19-532
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