衍生化-UPLC-MS／MS法测定面粉中的偶氮甲酰胺  

Determination of Azodicarbonamide in Flour by UPLC-MS/MS After Derivatization

作　　者：马立利[1] 曹沅[1] 胡艳霞 曹英华[1] 贾丽[1] 范筱京[1] 

机构地区：[1]北京市理化分析测试中心北京市食品安全分析测试工程技术研究中心,北京100089 [2]华北制药集团爱诺有限公司,石家庄052165

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

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.

关 键 词：面粉 偶氮甲酰胺(ADA) 氨基脲(SEM) 超高效液相色谱-串联质谱联用(UPLC—MS/MS) 

分 类 号：TS211.4[轻工技术与工程—粮食、油脂及植物蛋白工程]