| 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 |
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| 引用本文： | 朱铭立,杨黎忠,张卫锋,蔡成元,周向东.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[J].色谱,2019,37(2):189-193. |
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| 作者姓名： | 朱铭立 杨黎忠 张卫锋 蔡成元 周向东 |
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| 作者单位： | 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 |
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| 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。
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| 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 |
| 收稿时间： | 2018-10-26 |
Determination of acrylamide in coffee by ultra performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry |
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| ZHU Mingli,YANG Lizhong,ZHANG Weifeng,CAI Chengyuan,ZHOU Xiangdong.Determination of acrylamide in coffee by ultra performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry[J].Chinese Journal of Chromatography,2019,37(2):189-193. |
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| Authors: | ZHU Mingli YANG Lizhong ZHANG Weifeng CAI Chengyuan ZHOU Xiangdong |
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| Affiliation: | 1. Guangzhou Agricultural Products Quantity and Safety Supervisory Institute, Guangzhou 510308, China;
2. PerkinElmer Management(Shanghai) Co., Ltd, Shanghai 201203, China |
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| 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. |
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| Keywords: | ultra performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (UHPLC-APCI-MS/MS) acrylamide coffee |
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