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目的建立超高效液相色谱-串联质谱法测定面制品中的氨基脲含量,并研究偶氮甲酰胺添加水平对面粉中氨基脲含量的影响及两者的转化条件。方法样品经盐酸水解、邻硝基苯甲醛衍生、HLB小柱净化及乙酸乙酯提取;质谱以电喷雾电离源正离子模式扫描监测,用带有同位素内标的衍生物~(15)N_2~(13)C-SEM-NBA定量检测目标氨基脲衍生物。结果氨基脲在0.5~100μg/kg范围内呈良好线性关系,相关系数为0.9995,检出限为0.5μg/kg,加标回收率在85.1%~114.6%之间,相对标准偏差为3.2%~6.9%。市售10份面制品中氨基脲的阳性检出率为41.7%。氨基脲是偶氮甲酰胺在湿热的条件下生成的,并且同一种面制品中外部氨基脲含量比内部含量大。结论本方法快速、准确且灵敏度高,可适用于面制品中氨基脲的定量分析。
OBJECTIVE To establish a method for the determination of semicarbazide in flour products by ultra performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) and to study the influence of the azodicarbonamide level on the content of semicarbazide in flour and the conversion conditions. Methods The sample was hydrolyzed by hydrochloric acid, o-nitrobenzaldehyde, purified by HLB cartridge and extracted with ethyl acetate. Mass spectrometry was monitored by electrospray ionization source positive ion mode scanning. The isotope internal standard derivative ~ (15) N 2 ~ ( 13) C-SEM-NBA Quantification of target semicarbazide derivatives. Results The semicarbazide showed a good linearity in the range of 0.5-100 μg / kg with a correlation coefficient of 0.9995. The detection limit was 0.5 μg / kg. The recoveries were within the range of 85.1% -114.6%. The relative standard deviations were 3.2% 6.9%. The positive detection rate of semicarbazide in the 10 commercially available noodle products was 41.7%. Semicarbazide is azodicarbonamide generated under hot and humid conditions, and the same type of surface preparation of semicarbazide content than the internal content. Conclusion The method is rapid, accurate and sensitive and can be applied to the quantitative analysis of semicarbazide in flour products.