乳及乳制品中三聚氰胺的含量.PDFVIP

※分析检测 食品科学 2012, Vol.33, No.20 171 HPLC-PADUPLC-MS/MS 1 2 1 1 1,* 单 艺 ，马 微 ，王象欣 ，鄂来明 ，姜毓君 (1.东北农业大学 黑龙江省乳品工业技术开发中心，黑龙江 哈尔滨 150086 ； 2.黑龙江出入境检验检疫局，黑龙江 哈尔滨 150001) 摘 要：分别建立高效液相色谱-二极管阵列法(HPLC-PAD)、超高压液相色谱- 串联质谱法(UPLC-MS/MS)测定乳及 乳制品中三聚氰胺含量的方法。利用HPLC-PAD外标法进行样品中三聚氰胺的初筛，利用UPLC-MS/MS法进行确 证，以13 15 C N -三聚氰胺为同位素内标定量。乳制品经乙腈、乙酸锌、盐酸溶液提取，质谱检测时，样品再经MCX 3 3 固相萃取柱富集净化。HPLC-PAD法的定量限为4mg/kg ，UPLC-MS/MS 的定量限为0.05mg/kg ；HPLC-PAD 的添加回 收率为95.7%～102.3%，UPLC-MS/MS 的添加回收率为91.3%～95.7%(基质匹配曲线校正) ，两种方法的相对标准偏 差(RSD)分别为1.98%～4.51% ，1.60%～3.27% 。 三聚氰胺；高效液相色谱；超高压液相色谱- 串联质谱；内标法；乳制品 HPLC-PAD with External Standard Quantifi cation and UPLC-MS/MS with Internal Standard Quantifi cation for the Determination of Melamine in Milk and Milk Products 1 2 1 1 1,* SHAN Yi ，MA Wei ，WANG Xiang-xin ，E Lai-ming ，JIANG Yu-jun (1. Heilongjiang Dairy Industry Technical Development Center, Northeast Agricultural University, Harbin 150086, China； 2. Heilongjiang Entry-Exit Inspection and Quarantine Bureau, Harbin 150001, China) Abstract ：A method for the determination of melamine in milk and milk products was established by joint use of HPLC-PAD with external standard quantifi cation and UPLC-MS/MS with internal standard quantifi cation. Melamine content of samples was primarily analyzed by HPLC-PAD with external standard quantifi cation, and then confi rmed by UPLC-MS/MS and quantifi ed by internal standard method using 13 15