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目的建立用超高效液相色谱-串联三重四级杆质谱仪(UPLC-MS/MS)检测小麦粉制品中的氨基脲的定性定量方法,并研究了偶氮甲酰胺添加水平对面包中氨基脲含量的影响及两者的转化条件。方法在偏酸性条件下将样品水解,经邻硝基苯甲醛衍生乙酸乙酯提取,采用电喷雾电离,正离子扫描,用带有同位素内标的衍生物15N132C-SEMNBA定量检测目标氨基脲衍生物,优化液相色谱质谱检测条件,内标法定量。结果氨基脲的浓度为0.5μg/kg~100μg/kg时,线性关系良好,线性方程为y=352x+383,相关系数(r)为0.999 5,检出限为0.5μg/kg,加标回收率为85.1%~114.6%,相对标准偏差(RSD)为3.2%~6.9%。市售面制品中氨基脲的阳性检出率为41.7%。结论本方法快速、准确、灵敏度高,适用于面制品中氨基脲的定量分析。实验证明氨基脲是偶氮甲酰胺在湿热的条件下生成的,并且同一种小麦粉制品中样品外部的氨基脲含量比内部含量大。
OBJECTIVE To establish a qualitative and quantitative method for the determination of semicarbazide in wheat flour products by ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry (UPLC-MS / MS), and to study the effects of azodicarbonamide level on the content of semicarbazide The impact of both and the conversion conditions. Methods The samples were hydrolyzed under acidic conditions, extracted with o-nitrobenzaldehyde and extracted with ethyl acetate. The target semicarbazide derivatives were quantitatively determined by electrospray ionization and positive ion scanning with 15N132C-SEMNBA with isotope internal standard. Optimization of liquid chromatography mass spectrometry detection conditions, internal standard method. Results When the concentration of semicarbazide was 0.5μg / kg ~ 100μg / kg, the linear relationship was good, the linear equation was y = 352x + 383, the correlation coefficient was 0.999 5, the detection limit was 0.5μg / kg, Rates ranged from 85.1% to 114.6% with relative standard deviations (RSDs) between 3.2% and 6.9%. The positive detection rate of semicarbazide in commercial noodles was 41.7%. Conclusion The method is rapid, accurate and sensitive and suitable for the quantitative analysis of semicarbazide in flour products. It has been experimentally proved that the semicarbazide is azodicarbonamide formed under hot and humid conditions, and the semicarbazide content outside the sample in the same wheat flour product is larger than the internal content.