QuEChERS-超高效液相色谱串联质谱法测定乳粉中的双氰胺.pdfVIP

现代食品科技 Modern Food Science and Technology 2013, Vol.29, No.5 QuEChERS-超高效液相色谱串联质谱法测定 乳粉中的双氰胺 罗海英，冼燕萍，侯向昶，吴文海，吴玉銮，郭新东，王莉 （广州市质量监督检测研究院，国家加工食品质量监督检验中心（广州），广州市食品安全检测技术重点实验室， 广州市食品安全风险动态监测与预警研究中心，广东广州 510110） 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25 µg/kg，其余4种样品均为12 µg/kg；添加水平为12~250 µg/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。 关键词：双氰胺；乳粉；超高效液相色谱串联质谱法；QuEChERS法 文章篇号：1673-9078(2013)5-1148-1153 Determination of Dicyandiamide in Milk Powder Samples by QuEChERS-Ultra-HPLC-Tandem MS LUO Hai-ying, XIAN Yan-ping, HOU Xiang-chang, WU Wen-hai, WU Yu-luan, GUO Xin-dong, WANG Li (Guangzhou Quality Supervision and Testing Institute, National Centre for Quality Supervision and Testing of Processed Food (Guangzhou), Guangzhou City Key Laboratory of Detection Technology for Food Safety, Guangzhou City Research Center of Risk Dynamic Detection and Early Warning for Food Safety, Guangzhou Guangdong 510110, China) Abstract: A new method was established to determine Dicyandiamide in milk powder samples by QuEChERS cleanup combined with ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The sample was dissolved and extracted in hot water through ultrasonic wave, and protein was precipitated in acetonitrile. 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 extern