超高效液相色谱-串联质谱联用检测面制品中氨基脲方法的研究

Study on determination methods of semicarbazide in flour products by ultra high performance liquid chromatography-tandem mass spectrometry

目的建立用超高效液相色谱一串联三重四级杆质谱仪(UPLC-MS/MS)测面制品中氨基脲的定性定量方法。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^(15)N_2^(13)C-SEM-NBA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:氨基脲在0.5~100μg/kg范围内呈良好线性,相关系数为0.999 5,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(RSD)为3.2%~6.9%。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。

[Objective]To develop a qualitative and quantitative method based on ultra high performance liquid chromatographytandem mass spectrometry（UPLC-MS/MS） for the determination of semicarbazide in flour products.[Methods]The samples were hydrolyzed under the acidic solution,derived by 2-NBA,and extracted by ethyl acetate.With the electrospray ionization and positive ion scanning,the target of semicarbazide derivatives was detected quantitatively by the derivative of^（15） N_2^（13） C-SEM-NBA with isotope internal standard.The detection conditions of liquid chromatography mass spectrometry were optimized,and quantification was obtained by internal standard.[Results]The linear range for semicarbazide was 0.5-100 μg/kg,with the correlation coefficient was 0.999 5,and the detection limit was 0.5 μg/kg.The recovery rates were 85.1%-114.6% and the RSD were 3.2%~6.9%.[Conclusion]This method is rapid,accurate and high sensitivity,which is suitable for quantitative analysis of semicarbazide in flour product.