摘要
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0.2～80μg/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。
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） from 0.97% to 1.95%. For mutton, average spike recoveries （6 replicates） at 3 levels ranged from 80.95% to 82.95%, with a RSD from 0.70% to 2.32%. The method proved to be rapid, accurate and reliable.
出处
《食品科学》
EI
CAS
CSCD
北大核心
2010年第10期196-199,共4页
Food Science
基金
教育部"留学回国人员科研启动基金"资助项目(教外司留[2009]1001号)
关键词
三聚氰胺
牛肉
羊肉
高效液相色谱
melamine
beef
mutton
high performance liquid chromatography
