色谱 ›› 2019, Vol. 37 ›› Issue (2): 189-193.DOI: 10.3724/SP.J.1123.2018.10038

• 研究论文 • 上一篇    下一篇

超高效液相色谱-大气压化学电离-串联质谱法测定烘焙咖啡中丙烯酰胺

朱铭立1, 杨黎忠2, 张卫锋1, 蔡成元2, 周向东2   

  1. 1. 广州市农产品质量安全监督所, 广东 广州 510308;
    2. 珀金埃尔默企业管理(上海)有限公司, 上海 201203
  • 收稿日期:2018-10-26 出版日期:2019-02-09 发布日期:2014-12-31
  • 通讯作者: 朱铭立,Tel:(020)32306524,E-mail:zhumingli0529@163.com

Determination of acrylamide in coffee by ultra performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry

ZHU Mingli1, YANG Lizhong2, ZHANG Weifeng1, CAI Chengyuan2, ZHOU Xiangdong2   

  1. 1. Guangzhou Agricultural Products Quantity and Safety Supervisory Institute, Guangzhou 510308, China;
    2. PerkinElmer Management(Shanghai) Co., Ltd, Shanghai 201203, China
  • Received:2018-10-26 Online:2019-02-09 Published:2014-12-31

摘要:

建立了烘焙咖啡中丙烯酰胺的超高效液相色谱-大气压化学电离-串联质谱(UHPLC-APCI-MS/MS)分析方法。样品经甲醇提取,HLB固相萃取(SPE)小柱净化,Brownlee validated AQ C18色谱柱分离,采用大气压化学电离(APCI)源,正离子扫描和多反应监测(MRM)模式对丙烯酰胺进行检测,内标法定量。结果表明,丙烯酰胺在0.5~100.0 μg/L范围内具有良好的线性关系,相关系数(r2)为0.999,方法检出限为5.0 μg/kg,定量限为10.0 μg/kg。在100.0、200.0和1000.0 μg/kg添加水平下,丙烯酰胺的回收率为94.6%~115.0%,相对标准偏差(RSD)值为2.8%~3.6%(n=6)。本方法采用APCI源作为离子化方式,能有效地减少咖啡基质对丙烯酰胺的基质干扰,前处理简单,灵敏度高,适用于咖啡中丙烯酰胺的日常检测。

关键词: 丙烯酰胺, 超高效液相色谱-大气压化学电离串联质谱, 咖啡

Abstract:

A method using ultra high performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (UHPLC-APCI-MS/MS) was developed for the determination of acrylamide in coffee. The coffee samples spiked with 13C3-acrylamide as the internal standard were extracted with methanol, and cleaned using HLB solid phase extraction (SPE) cartridges. The liquid chromatography separation was performed on a Brownlee validated AQ C18 column with isocratic elution. Methanol and 0.1% (volume percentage) formic acid aqueous solution were used as the mobile phase. Identification of acrylamide was achieved by APCI-MS/MS with multiple reaction monitoring (MRM) in the positive mode. The quantification analysis was performed by the internal standard method. The calibration curve showed good linearity with a correlation coefficient of 0.999 in the range of 0.5-100.0 μg/L. The limit of detection (LOD) was 5.0 μg/kg. The limit of quantification (LOQ) was 10.0 μg/kg. Recovery of acrylamide from coffee sample was evaluated at concentrations of 100.0, 200.0 and 1000.0 μg/kg. The average recoveries of acrylamide were between 94.6%-115.0% with relative standard derivations (RSDs) in the range of 2.8%-3.6% (n=6). This simple, accurate and sensitive method was proven to be suitable for the determination of acrylamide in coffee.

Key words: acrylamide, coffee, ultra performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (UHPLC-APCI-MS/MS)

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