色谱

色谱

• 研究论文 • 上一篇    下一篇

不粘锅涂层中全氟辛酸及其盐的快速溶剂萃取-气相色谱-质谱法测定

白桦,郝楠,崔艳妮,周新,蔡天培,张青,王超,王军兵   

  1. Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • 收稿日期:2006-08-30 修回日期:2006-12-22 出版日期:2007-03-30 发布日期:1985-12-25
  • 通讯作者: 白桦

Determination of Perfluorooctanoic Acid and Its Salts in the Coating Layer of Nonstick Pan by Gas Chromatography/Mass Spectrometry Coupled with Accelerated Solvent Extractor

BAI Hua, HAO Nan, CUI Yanni, ZHOU Xin, CAI Tianpei, ZHANG Qing, WANG Chao, WANG Junbing   

  1. Chinese Academy of Inspection and Quarantine, Beijing 100025, China
  • Received:2006-08-30 Revised:2006-12-22 Online:2007-03-30 Published:1985-12-25
  • Contact: BAI Hua

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摘要： 建立了不粘锅涂层中全氟辛酸(PFOA)及其盐残留量的气相色谱-负离子化学电离质谱（GC/NCI-MS）测定方法。样品经快速溶剂萃取仪提取及衍生化处理后进行GC/NCI-MS测定。PFOA的定量检测限为5 μg/kg;4个添加水平的平均回收率为90.9%~96.2%,相对标准偏差为1.37%~6.37%。该方法提取时间短,提取效率高,衍生化步骤简单,杂质干扰小,灵敏度高,适用性强。

关键词: 不粘锅涂层 , 快速溶剂萃取, 气相色谱/质谱法, 全氟辛酸及其盐

Abstract: A sensitive, accurate and reproducible analytical method was developed and validated to quantify perfluorooctanoic acid (PFOA) and its salts  in the coating layer of nonstick pan. Scraped samples of 0.5 gram were directly extracted with acetonitrile using an accelerated solvent extractor at 175 ℃, 10.3 MPa for 20 min. After rotary evaporation concentration, the PFOA was derivatized with acetyl chloride and methanol at 65 ℃ for 60 min in an air-tight container. An HP-1 MS capillary column (30 m×0.25 mm, 0.33 μm) was used for the separation of the analyte. The procedure for the analysis of PFOA was based on gas chromatography interfaced to negative chemical ion mass spectrometry, operated in selected ion monitoring mode. Selected ions of m/z 312, 350, 378, 408, 428 were chosen for quantitation. The assay was linear over the range of 0-1000 μg/L, and the detection limit of PFOA was 5 μg/kg. The precision and recovery were assessed on four different concentrations (5, 20, 100, 500 μg/kg). The recoveries were in the range of 90.9%-96.2% and the relative standard deviations were 1.37%-6.37%. The procedure was applied to monitoring PFOA in the coating layer of nonstick pan from supermarket and no positive result was found.

Key words: accelerated solvent extraction （ASE）, coating layer of nonstick pan , perfluorooctanoic acid and its salts, gas chromatography/mass spectrometry (GC/MS)