超高效液相色谱-串联质谱法测定面粉中的偶氮甲酰胺

Determination of Azodicarbonamide in Flour by UPLC-MS/MS

摘要:

本文建立了面粉中偶氮甲酰胺(ADA)的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。面粉样品中的ADA经湿热处理后，最终转变成氨基脲(SEM)，加入2-硝基苯甲醛37 ℃过夜衍生化，乙酸乙酯提取后，电喷雾正离子扫描，多反应监测(MRM)模式检测，外标法定量，通过测定SEM的量来间接计算ADA含量。该方法的ADA检测限为0.21 mg/kg，远远低于HPLC法的1 mg/kg；线性范围为1~100 mg/kg，相关系数r=0.9997，回收率为86.8~117.2%，相对标准偏差(RSD)<6%。该方法方便、灵敏度高、定性定量准确，可实现对面粉中偶氮甲酰胺的检测。

Abstract:

A quantitative assay for the determination of azodicarbonamide(ADA) using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed. ADA in flour was hydrolyzed with wet heat processing and formed semicarbazide (SEM) finally. SEM was derivatized overnight with 2-nitrobenzaldenhyde at 37 ℃. The derivative was extracted with ethyl acetate, and MS detection was performed with the positive ion mode in multi-reaction monitoring (MRM). Determination of ADA was according to the amount of SEM which was determined as external method. Compared with the method of HPLC, the limit of detection was 0.21 mg/kg for ADA, which was lower than 1mg/kg for HPLC. Within the linear range of 1~100 mg/kg, correlation coefficient was 0.9997. The recovery rate were 86.8~117.2% (RSD <8%). The method developed was convenient, accuracy, and sensitivity to be used effectively for determining ADA in flour.