食品科学 ›› 2010, Vol. 31 ›› Issue (4): 201-205.doi: 10.7506/spkx1002-6300-201004046

• 分析检测 • 上一篇    下一篇

大米蛋白粉中三聚氰酸及其类似物的硅烷衍生化GC-MS检测方法研究

左海根   

  1. 江西出入境检验检疫局
  • 收稿日期:2009-06-02 修回日期:2009-11-12 出版日期:2010-02-15 发布日期:2010-12-29
  • 通讯作者: 左海根 E-mail:genzh@163.com

Silylation Followed by GC-MS Determination of Melamine and Its Analogues in Rice Protein Powder

ZUO Hai-gen   

  1. Jiangxi Entry-Exit Inspection and Quarantine Bureau, Nanchang 330002, China
  • Received:2009-06-02 Revised:2009-11-12 Online:2010-02-15 Published:2010-12-29
  • Contact: ZUO Hai-gen E-mail:genzh@163.com

摘要:

建立一种简单、快速、准确同时测定大米蛋白粉中三聚氰胺及其类似物三聚氰酸、三聚氰胺一酰胺、三聚氰胺二酰胺的方法。样品经二乙胺- 水- 乙腈(1:4:5,V/V)超声提取30min 后,提取液于70℃条件下氮气吹干,在吡啶介质中经甲基硅烷化衍生后采用气相色谱- 质谱仪测定(内标法定量)。此方法检测限为0.5mg/kg、线性相关系数(20~1000μg/L 范围内)不小于0.9989;当加标量为1.0~5.0mg/kg 时,平均回收率为72.01%~96.45%、相对标准偏差不大于6.3%。此方法可用于大米蛋白粉中三聚氰酸及其类似物的检测。

关键词: 气相色谱- 质谱联用, 三聚氰胺, 三聚氰胺一酰胺, 三聚氰胺二酰胺, 三聚氰酸

Abstract:

A GC-MS method was developed for the determination of melamine and its analogues in rice protein powder, like ammeline, ammelide and cyanuric acid. Samples were extracted with a mixture composed of diethylamine, water and acetonitrile (1:4:5, V/V) for 30 min, and the resulting extract was blown to dryness under dry nitrogen atmosphere at 70 ℃. Subsequently, the residue left was dissolved in pyridine and silylated for 40 min at 70 ℃ prior to GC-MS analysis. The internal standard method was used for quantification. Melamine and its analogues all exhibited a good linear curve over the concentration range of 20-1000 μg/L (r≥0.9989). The limit of detection (LOD) of the developed method was 0.5 mg/kg. Mean recoveries of melamine and its analogues at three spike levels of 1.0, 2.0 mg/kg and 5.0 mg/kg were between 72.01%-96.45%, with relative standard deviations (RSDs) not more than 6.3%. These figures of merit of this method demonstrate its good applicability to the determination of melamine and its analogues in rice protein powder.

Key words: GC-MS, melamine, ammeline, ammelide, cyanuric acid

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