摘要
建立了QuEChERS净化-超高效液相色谱串联三重四极杆质谱(UPLC-MS/MS)测定乳粉中双氰胺的新方法。样品用热水溶解和提取,乙腈沉淀蛋白,正己烷脱脂,QuEChERS净化,UPLC-MS/MS检测,以保留时间和特征离子对比例定性,外标法定量。探讨了脱脂乳粉、全脂乳粉、配方乳粉、酸乳粉和乳清粉5种样品的试验情况。结果表明,双氰胺在一定浓度范围内线性关系良好;方法定量限(S/N=10):配方乳粉为25μg/kg,其余4种样品均为12μg/kg;添加水平为12-250μg/k时,平均回收率在88.6-111%;相对标准偏差(n=6)为3.1-8.2%;日间精密度(n=5)为3.7-9.4%。应用本方法分析了25个样品,其中2个样品呈阳性。本方法具有前处理简单、准确、回收率高等特点,适用于不同乳粉样品中双氰胺的测定。
A new method was established to determine Dicyandiamide in milk powder samples by QuEChERS cleanup combined with nitro-high performance liquid chromatography tandem mass spectrometry （UPLC-MS/MS）. The sample was dissolved and extracted in hot water through ulWasonic wave, and protein was precipitated in acetonilrile. Then the extracted solution was purified by N-hexane and QuEChERS, and analyzed using UPLC-MS/MS. Dicyandiamide was identified by retention time and the ratio of the characteristic ions, and quantitatived with external standard method. In the study, the test situation and matrix effects of different samples matrix, including skimmed milk powder, whole milk powder, formula milk powder, acid milk powder and whey powder, were investigated. The result showed that the method quantitation limit （S/N=10） of dicyandiamide were 25 μg/kg in sample of formula milk powder and 12 μg/kg in the rest 4 kinds of sample. The average recoveries were between 88.6% and 111% at spiked levels of 12 - 250 ~g/kg, the precision （n=6） ranged from 3.1% to 8.2%. The inter-day RSDs （n=5） were between 3.7% and 9.4%. Among 25 samples analyzed, only 2 samples were positive. The method was simple, sensitive, and accurate for the determination of dicyandiamide in milk powder samples.
出处
《现代食品科技》
EI
CAS
北大核心
2013年第5期1148-1153,共6页
Modern Food Science and Technology
基金
广州市科技计划项目([2011]233-34,11C13190775)
关键词
双氰胺
乳粉
超高效液相色谱串联质谱法
QuEChERS法
dicyandiamide
milk powder samples
ultra-high performance liquid chromatography tandem mass spectrometry
QuEChERS
作者简介
罗海英（1976-），高工，主要从事食品安全检测技术研究工作
通讯作者：吴玉銮，教授级离工
