固相萃取-超高效液相色谱-串联质谱法检测面粉及面制品中的氨基脲  

Determination of semicarbazide in flour and flour products by SPE purification ultra-high performance liquid chromatography-tandem triple quadruple mass spectrometry

作　　者：王丹[1] 陈颖[1] 宋书锋[1] 高洁[1] 梁江[1] 赵云峰[1] 

机构地区：[1]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京10021

出　　处：《中国食品卫生杂志》2014年第6期579-583,共5页Chinese Journal of Food Hygiene

基　　金：973"食品加工过程安全性评价及危害物风险评估"(2012CB720804)

摘　　要：目的建立面粉及面制品中氨基脲的超高效液相色谱-三重四级杆串联质谱方法。方法在样品中加入同位素取代的氨基脲,以0.2 mol/L HCl提取后,与衍生剂邻硝基苯甲醛反应。衍生产物在中性条件下经HLB柱净化,乙酸乙酯洗脱,吹干复溶后,以超高效液相色谱的C18柱（50 mm×2.1 mm,1.7μm）分离,质谱法检测。以保留时间与质谱离子对定性,内标法定量。结果氨基脲在0.5~100μg/kg范围内呈线性相关。方法精密度良好（RSD〈20%,n=6）,回收率在60%~120%之间,定量限为0.5μg/kg（S/N=10）。结论本方法特异性强,灵敏度高,适合于面粉及面制品中的氨基脲检测。Objective An ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry（ UPLCMS / MS） method was developed for the determination of emicarbazide（ SEM） in flour and flour products. MethodsStable isotope labeled internal standard was added to the sample and SEM reacted with o-nitrobenzaldehyde in 0. 2 mol / L HCl to produce stable derivatization. The derivatization was cleaned up with HLB SPE cartridge,eluted with ethyl acetate,dried with nitrogen,and redissolved with 0. 1% formic acid. The sample was separated on a waters BEH C18 column. The detection was performed with waters Xevo TQ-S using postive electrospray ionization mode and multiple-reaction monitoring mode. Results The results showed that the linear range for SEM was 0. 5-100 μg / kg in flour. The method showed good accuracy with RSD 20%（ n = 6） and recovery in between 60% to 120%. Conclusion This method is fast,simple and has good reproducibility. It is suitable for semicarbazide determination in flour and flour products.

关 键 词：氨基脲 SPE纯化 超高效液相色谱-串联三重四极杆质谱法 面粉与面制品 食品污染物 食品安全 

分 类 号：O657.63[理学—分析化学] TS213.2[理学—化学]