高效液相色谱-串联质谱法测定生鲜乳中三聚氰胺的含量  

Determination of Melamine Residue in Milk by HPLC-MS/MS

作　　者：初晓娜 矫秀燕 穆阿丽 吴燕 耿勋 李辉 付红蕾 李彦 

机构地区：[1]青岛市饲料兽药检测站,青岛266071

出　　处：《理化检验（化学分册）》2015年第3期394-397,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：青岛市公共领域科技支撑计划项目(09-1-1-93-nsh)

摘　　要：采用高效液相色谱-串联质谱法测定生鲜乳中三聚氰胺残留量。样品经乙腈溶液超声提取,过Waters Oasis MCX固相萃取小柱净化,50℃氮气吹干,再用1.0mL乙腈溶解后供高效液相色谱-串联质谱分析。以Waters Hilic色谱柱(100 mm×2.1 mm,3μm)为固定相,用乙腈-5mmol·L-1乙酸铵(95+5)溶液洗脱,采用电喷雾正离子模式多反应监测,内标法定量。三聚氰胺的质量浓度在10.0μg·L-1以内呈线性,检出限(3S/N)为0.5μg·kg-1。取空白样品在3个标准加入水平下进行回收和精密度试验,回收率在99.8%~103%之间,测定值的相对标准偏差(n=10)在1.9%~3.2%之间。HPLC-MS/MS was applied to measure melamine residue in milk.The sample was extracted with acetonitrile-water,purified by Waters Oasis MCX solid phase extraction column,dried by nitrogen at 50 ℃,dissolved with 1mL of acetonitrile and used for HPLC-MS/MS analysis.Waters Hilic column(100mm×2.1mm,3μm)was used as stationary phase,and a mixture(95+5)of acetonitrile and 5mmol·L-1 of ammonium acetate as mobile phase.ESI+and MRM were adopted in MS/MS.Internal standard method was used for quantization.Linearity range of melamine was within 10.0μg·L-1,the detection limit(3S/N)was 0.5μg·kg-1.Tests for recovery and precision were made by addition of melamine,giving values of recovery in the range of 99.8%-103%and values of RSD′s(n=10)in the range of 1.9%-3.2%.

关 键 词：高效液相色谱-串联质谱法 内标 三聚氰胺 生鲜乳 固相萃取 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]