色谱

色谱 ›› 2013, Vol. 31 ›› Issue (5): 477-480.DOI: 10.3724/SP.J.1123.2012.11008

• 技术与应用 • 上一篇    下一篇

气相色谱-质谱联用法同时测定乳及乳制品中的三聚氰胺及肌酐

曾凯1*, 刘峙嵘2, 宁雅君1, 李金林1, 唐俊1, 张敏1   

  1. 1. 南昌市食品质量卫生安全监督检验中心, 江西 南昌 330012;
    2. 东华理工大学, 江西 抚州 344000
  • 收稿日期:2012-11-19 修回日期:2013-01-23 出版日期:2013-05-28 发布日期:2013-05-16
  • 通讯作者: 曾凯,Tel:(0791)88119861,E-mail:zk19831125@163.com.
  • 基金资助:

    江西省质量技术监督局科技项目(GZJK201102).

Simultaneous determination of melamine and creatinine in milk and milk products by gas chromatography-mass spectrometry

ZENG Kai1*, LIU Zhirong2, NING Yajun1, LI Jinlin1, TANG Jun1, ZHANG Min1   

  1. 1. Nanchang Food Quality Health Safety Supervision and Inspection Center, Nanchang 330012, China;
    2. East China Institute of Technology, Fuzhou 344000, China
  • Received:2012-11-19 Revised:2013-01-23 Online:2013-05-28 Published:2013-05-16

PDF

195

被引次数

5

摘要：

建立了同时测定乳制品中三聚氰胺及肌酐的气相色谱-质谱联用方法。样品经1%三氯乙酸溶液萃取,混合型阳离子交换固相萃取净化,提取液用氮气吹干后加入N,O-双(三甲基硅基)三氟乙酰胺-三甲基氯硅烷(BSTFA-TMCS)硅烷化试剂,于75 ℃下衍生60 min,最后采用选择离子模式下的气相色谱-质谱测定。三聚氰胺和肌酐的定量限分别为0.10 mg/kg和0.20 mg/kg;在0.1～50 mg/L范围内的线性相关系数均大于0.99。实际样品中,肌酐在10～100 mg/kg和三聚氰胺在0.1～5.0 mg/kg添加范围内的回收率分别为80.7%～116.8%和77.6%～107.5%,相对标准偏差分别小于9.4%和8.5%。该方法能有效除去干扰,灵敏度高,回收率较好,可用于乳制品中三聚氰胺和肌酐的同时测定。

关键词: 肌酐, 气相色谱-质谱联用, 乳, 乳制品, 三聚氰胺

Abstract:

A method established for determining melamine and creatinine in milk and milk products. The samples were extracted with 1% trichloracetic acid solution. The extract was cleaned-up by using a mixed-mode cation ion exchange SPE column and evaporated to dryness under nitrogen. The residue was derived by bis(trimethylsilyl)trifluoroacetamide-chlorotrimethylsilane (BSTFA-TMCS), then determined by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. Melamine and creatinine had good linearity in the range of 0.1-50 mg/L with the correlation coefficients higher than 0.99, and the limits of quantification were 0.10 mg/kg and 0.20 mg/kg, respectively. The recoveries of melamine and creatinine were 80.7%-116.8% and 77.6%-107.5% with RSD no more than 9.4% and 8.5% in the spiked range of 10-100 mg/kg and 0.1-5.0 mg/kg, respectively. The method is accurate, sensitive, and suitable for the determination of creatinine in milk and milk products.

Key words: creatinine, gas chromatography-mass spectrometry (GC-MS), melamine, milk, milk products

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