偶氮二甲酰胺(ADA)由于其氧化和漂白特性而被批准为面粉产品中的食品添加剂。然而,由于其毒性和引起人类哮喘的风险,在澳大利亚和欧洲被禁止。开发了一种测定实际面粉样品中ADA的方法。这项工作提出了一种基于衍生化和清理程序的优化方法,然后是超高效液相色谱与电喷雾电离串联质谱(UPLC-ESI-MS/MS)。该分析方法已成功验证。在0.10-80mg/kg的浓度范围内,基质匹配的校准曲线的线性(R2>0.99)获得了出色的结果。回收率从81.7%到102.3%不等。重复性(n=6)的相对标准偏差(RSD)为1.3-4.1%,日间RSD(n=6)为2.2-4.8%。检出限和定量限分别为0.014和0.042mg/kg,显著低于中国食品安全国家标准(GB2760-2014)规定的45mg/kg的要求。26份面粉样品中ADA的检出率为23.1%,浓度范围为0.023至23.2mg/kg。
Azodicarbonamide (ADA) is approved as a food additive in flour products due to its oxidising and bleaching properties. However, it is prohibited in Australia and Europe on account of its toxicity and the risk of causing asthma in humans. A method was developed to determine ADA in actual flour samples. This work presents an optimised methodology based on derivatisation and clean-up procedures followed by ultra-performance liquid chromatography coupled with electrospray ionisation tandem mass spectrometry (UPLC-ESI-MS/MS). The analytical method was successfully validated. An excellent result was obtained for the linearity of matrix-matched calibration curves (R2 > 0.99) in the concentration range of 0.10-80 mg/kg. The recovery rate varied from 81.7% to 102.3%. The relative standard deviations (RSDs) of repeatability (n = 6) were 1.3-4.1%, and inter-day RSDs (n = 6) were 2.2-4.8%. The limit of detection and the limit of quantification were 0.014 and 0.042 mg/kg, which were significantly lower than the requirement of 45 mg/kg stipulated in the Chinese National Food Safety Standard (GB 2760-2014). The detection rate of ADA in 26 flour samples was 23.1%, with the concentration ranging from 0.023 to 23.2 mg/kg.