色谱

色谱

• 技术与应用 • 上一篇    下一篇

混合型固相萃取柱净化-气相色谱-质谱法测定婴幼儿配方奶粉中的三聚氰酸

李锋格*, 姚伟琴, 田延河, 窦辉, 苏敏, 朱慧萍, 李欣, 沈梦圆   

  1. 新疆出入境检验检疫局技术中心, 新疆 乌鲁木齐 830063
  • 收稿日期:2009-08-10 修回日期:2009-10-10 出版日期:2010-03-28 发布日期:1981-03-25
  • 通讯作者: 李锋格

Determination and confirmation of cyanuric acid ininfant formula using mixed-mode solid-phase extraction cartridge clean up-gas chromatography-mass spectrometry

LI Fengge*, YAO Weiqin, TIAN Yanhe, DOU Hui, SU Min, ZHU Huiping, LI Xin, SHEN Mengyuan   

  1. Technical Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China
  • Received:2009-08-10 Revised:2009-10-10 Online:2010-03-28 Published:1981-03-25
  • Contact: LI Fengge

PDF

553

被引次数

30

摘要： 建立了一种混合型固相萃取柱净化-气相色谱-质谱法(GC-MS)测定婴幼儿配方奶粉中三聚氰酸的方法。在84 ℃条件下,用0.5%乙酸水溶液提取样品中的三聚氰酸,离心,滤液经Carb/C18混合型固相萃取柱净化,氮气吹干,硅烷化衍生,GC-MS测定,选择离子监测模式,外标法定量。在0.01～2 mg/L内线性关系良好(r＞0.99),在0.25～2.5 mg/kg的添加水平范围内,平均回收率为80%～103%,相对标准偏差(RSD)为7.7%～14.5%,三聚氰酸的检出限(LOD)为0.10 mg/kg,定量限(LOQ)为0.25 mg/kg。该方法快速、灵敏、准确、专一、耐用,适合婴幼儿配方奶粉中三聚氰酸的确证和定量测定。

关键词: 混合型固相萃取柱净化, 气相色谱-质谱, 三聚氰酸, 婴幼儿配方奶粉

Abstract: A method is presented for the quantitative determination and confirmation of cyanuric acid in infant formula by mixed-mode solid-phase extraction cartridge clean up-gas chromatography-mass spectrometry (GC-MS). Cyanuric acid was extracted from infant formula with an acetic acid solution at 84 ℃. An aliquot of the supernatant was cleaned up using mixed-mode solid-phase extraction cartridge containing C18 and graphitized carbon black (GCB), and evaporated to dryness under nitrogen. The residues were converted to trimethylsilyl derivatives, then determined by GC-MS in selected ion monitoring (SIM) mode. The linear range was from 0.01－2 mg/L. The recoveries were 80%－103% and the relative standard deviations were 7.7%－14.5% in the spiked range of 0.25－2.5 mg/kg. The limit of detection was 0.10 mg/kg and the limit of quantification was 0.25 mg/kg. The method is rapid, sensitive, accurate, specific, and rugged. It is suitable for the quantitative determination and confirmation of cyanuric acid in infant formula.

Key words: cyanuric acid, infant formula , mixed-mode solid-phase extraction cartridge clean up, gas chromatography-mass spectrometry(GC-MS)