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）分析方法。面粉经湿热处理，ADA转化为氨基脲（SEM），加入内标溶液和2-硝基苯甲醛后衍生化，经HLB固相萃取柱净化后，乙酸乙酯洗脱，采用电喷雾正离子模式（ESI＋）检测，内标法定量，通过测定SEM衍生物的量间接计算面粉中ADA的含量。该方法的定量限为0．4mg／kg；在0．2-5mg／kg浓度范围内，尼。大于0．99；添加浓度为0．4mg／kg、0．8mg／kg、4．0mg／kg时，回收率为89．2％-116．7％，RsD为7．8％-15．2％。该方法灵敏度高，定性定量准确，适宜于面粉中偶氮甲酰胺的分析检测。
An ultrahigh performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method was developed for the determination of azodicarbonamide （ADA） in flour after wet heat processing and derivatization with 2-nitrobenzaldenhyde. The derivatized samples were purified by Oasis HLB solid phase extraction cartridges, then was analyzed by UPLC-MS/MS with electrospray ionization, operated under positive ion mode. ADA in flour was quantified according to the amount of SEM by internal standard method. The limit of quantification was 0.4 mg/kg, and a good linearity of calibration curve was obtained in the range of 0.2-5 mg/kg with the linear regression coefficients （RE） higher than 0.99. Average recoveries for spiked samples at 0.4 mg/kg, 0.Smg/kg, and 4.0mg/kg were in the range from 89.2% to 116.7% with RSDs from 7.8% to 13.2%. The method is reliable, high sensitive, and accurate to be used for determining ADA in flour.
出处
《现代科学仪器》
2016年第5期78-82,共5页
Modern Scientific Instruments
基金
北京市财政资金项目创新工程III-1（PXM2015_178305_000001）资助
