食品科学 ›› 2010, Vol. 31 ›› Issue (10): 196-199.doi: 10.7506/spkx1002-6630-201010040

• 分析检测 • 上一篇    下一篇

牛羊肉中三聚氰胺的HPLC快速检测

李巧玲1,安源2,张艳川1,杨金1   

  1. 1. 河北科技大学生物科学与工程学院
    2. 长春大学生物科学技术学院
  • 收稿日期:2009-08-10 修回日期:2009-12-04 出版日期:2010-05-15 发布日期:2010-12-29
  • 通讯作者: 李巧玲 E-mail:lql98119@126.com
  • 基金资助:

    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)

Rapid HPLC Determination of Melamine in Beef and Mutton

LI Qiao-ling1,AN Yuan2,ZHANG Yan-chuan1,YANG Jin1   

  1. 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
  • Received:2009-08-10 Revised:2009-12-04 Online:2010-05-15 Published:2010-12-29
  • Contact: LI Qiao-ling E-mail:lql98119@126.com

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。

关键词: 三聚氰胺, 牛肉, 羊肉, 高效液相色谱

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) 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.

Key words: melamine, beef, mutton, high performance liquid chromatography

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