牛羊肉中三聚氰胺的 HPLC 快速检测.PDFVIP

196 2010, Vol. 31, No. 10 食品科学 ※分析检测 1 2 1 1 李巧玲 ，安 源 ，张艳川 ，杨 金 (1.河北科技大学生物科学与工程学院，河北石家庄 050018 ；2.长春大学生物科学技术学院，吉林长春 130012) 建立高效液相色谱(HPLC)检测牛、羊肉中三聚氰胺的检测方法。样品经1% 三氯乙酸- 乙腈(3:1 ，V/V)提 取，利用阳离子交换固相萃取柱净化后，洗脱液于50 ℃条件下用氮气吹干，残渣用离子对试剂缓冲液- 乙腈(90: 10，V/V)溶解，用高效液相色谱法由紫外检测器检测、外标法定量。结果表明，三聚氰胺在0.2～80 μg/mL 质量 浓度范围内具有良好的线性关系，线性相关系数(R2) 为0.9999 ，其检出限为0.05mg/kg 。在牛肉样品中，三聚氰胺 的平均回收率为81.73%～83.35% ，相对标准偏差为0.97% ～1.95%；在羊肉样品中，三聚氰胺的平均回收率为 80.95% ～82.95% ，相对标准偏差为0.70% ～2.32% 。本方法具有操作快捷、灵敏度高、重现性好等优点。 ：三聚氰胺；牛肉；羊肉；高效液相色谱 Rapid HPLC Determination of Melamine in Beef and Mutton 1 2 1 1 LI Qiao-ling ，AN Yuan ，ZHANG Yan-chuan ，YANG Jin (1. College of Bioscience and Bioengineering, Hebei University of Science and Technology, Shijiazhuang 050018, China； 2. Biological Scientific and Technical College, Changchun University, Changchun 130012, China) Abstract：A rapid HPLC method was developed for the determination of melamine in beef and mutton. Samples were extracted with a mixture of trichloroacetic acid and acetonitrile mixture (3:1 ，V/V) and cleaned up on a cation exchange solid-phase extraction (SPE) column. The eluate was blown to dryness under nitrogen at 50 ℃ and then dissolved in a mixture of ion-pair buffer and acetonitrle (90:10, V/V). The analysis was carried out using HPLC with UV detector. A good linear relationship was observed for melamine within the range of 0.2 －80 μg/mL and the linear correlation coefficient (R2) was 0.9999. The limit of detection was 0.05 mg/kg. For beef, average spike recoveries (6 replicates) at 3 levels ranged from 81.73% to 83.35%, with a relative standard deviation (RSD) fro