色谱法
化学
分析物
固相萃取
质谱法
选择性反应监测
液相色谱-质谱法
电喷雾电离
硝基呋喃
萃取(化学)
检出限
高效液相色谱法
电喷雾
样品制备
串联质谱法
甲酸
生物
遗传学
作者
Rui Chen,Jiaxuan Li,Zhiwei Yang,Xiang Li,Fengmei Zhu,Jun Li,Jinjie Zhang
出处
期刊:Journal of Food Protection
[International Association for Food Protection]
日期:2020-05-01
卷期号:83 (5): 910-914
被引量:2
摘要
3,5-Dinitrosalicylic acid hydrazide (DNSAH) is the metabolite of the antibacterial nitrofuran nifursol. A simple and accurate analytical method to determine DNSAH levels in honey by solid-phase extraction-ultraperformance liquid chromatography-tandem mass spectrometry 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 with an electrospray ionization source and multiple reaction monitoring mode and was quantified by the internal standard method. The detection and quantitative limits 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 approximately 0.1 to 200 μg/L, with the correlation coefficient >0.9991. Under the concentration levels of 0.2, 0.5, 1.0, and 2.0 μg/kg, the average recovery rate were between 98.5 and 102.3%, and the relative standard deviations were between 1.1 and 5.4%. The results indicate that the method is simple, rapid, sensitive, and reproducible and can be used to determine DNSAH levels in different types of honey.
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