色谱

色谱 ›› 2013, Vol. 31 ›› Issue (11): 1129-1133.DOI: 10.3724/SP.J.1123.2013.06006

• 技术与应用 • 上一篇    下一篇

气相色谱-三重四极杆串联质谱法同时测定调味品中的氨基甲酸乙酯和氯丙醇

徐小民1, 何华丽2, 阮宇迪2, 黄百芬1, 张京顺1, 蔡增轩1, 任一平1   

  1. 1. 浙江省疾病预防控制中心, 浙江 杭州 310051;
    2. 浙江工业大学化学工程与材料科学学院, 浙江 杭州 310014
  • 收稿日期:2013-06-03 修回日期:2013-07-10 出版日期:2013-11-28 发布日期:2013-12-05
  • 通讯作者: 任一平
  • 基金资助:

    浙江省分析测试基金项目(04016);浙江省重点科技创新团队计划项目(2011R50021).

Simultaneous determination of ethyl carbamate and chloropropanols in flavorings by gas chromatography- triple quadrupole tandem mass spectrometry

XU Xiaomin1, HE Huali2, RUAN Yudi2, HUANG Baifen1, ZHANG Jingshun1, CAI Zengxuan1, REN Yiping1   

  1. 1. Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou 310051, China;
    2. College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, China
  • Received:2013-06-03 Revised:2013-07-10 Online:2013-11-28 Published:2013-12-05

PDF

387

被引次数

4

摘要：

建立了气相色谱-三重四极杆串联质谱(GC-MS/MS)同时测定调味品中氨基甲酸乙酯(EC)和氯丙醇(3-氯-1,2-丙二醇(3-MCPD)和2-氯-1,3-丙二醇(2-MCPD))的方法。样品添加同位素内标后,采用ExtrelutTM NT有机硅藻土填料进行基质固相分散萃取,先用正己烷淋洗除杂,再用乙酸乙酯-乙醚(20:80, v/v)混合溶剂洗脱被测物,洗脱液经浓缩后采用GC-MS/MS多反应监测(MRM)模式测定。EC、3-MCPD和2-MCPD的方法检出限依次为2、5和5 μg/kg,线性范围依次为5~1000 μg/kg(r=0.9997)、10~1000 μg/kg(r=0.9991)和10~1000 μg/kg(r=0.9995)。酱油、料酒(黄酒)、沙拉酱和方便面调味料4种基体中在20、100和400 μg/kg 3个水平加标测定的平均回收率和相对标准偏差(RSD,n=7)范围分别为EC: 87.7%~104%(RSD为4.3%~10.7%)、3-MCPD: 90.1%~109%(RSD为2.6%~10.2%)、2-MCPD: 90.9%~103%(RSD为3.0%~9.5%)。在部分酱油、料酒和方便面调味料中同时检测到了EC、3-MCPD和2-MCPD,在部分沙拉酱中检测到了EC或3-MCPD。该法准确、快速,适用于调味品中EC、3-MCPD和2-MCPD的同时检测。

关键词: 氨基甲酸乙酯, 调味品, 氯丙醇, 气相色谱-三重四极杆串联质谱, 同位素内标法

Abstract:

A simultaneous determination method for ethyl carbamate (EC) and chloropropanols (3-monochloropropane-1,2-diol (3-MCPD) and 2-monochloropropane-1,3-diol (2-MCPD)) in flavorings was developed by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). After spiked with internal standard, the sample was extracted by matrix solid-phase dispersion extraction technique with an ExtrelutTM NT column. Hexane was used to wash the fat soluble matrix interferences and then an ethyl acetate-ethyl ether (20:80, v/v) mixture was added to elute the analytes. The concentrated extract was detected by GC-MS/MS in multiple reaction monitoring (MRM) mode. The limits of detection (LODs) were 2, 5 and 5 μg/kg for EC, 3-MCPD and 2-MCPD, respectively. The linear ranges were 5-1000 μg/kg (r=0.9997), 10-1000 μg/kg (r=0.9991) and 10-1000 μg/kg (r=0.9995) for EC, 3-MCPD and 2-MCPD, respectively. In soy sauce, yellow rice wine, salami sauce and flavoring of instant noodle matrices, the recoveries (RSDs, n=7) in MRM mode at the levels of 20, 100 and 400 μg/kg were 87.7%-104% (4.3%-10.7%), 90.1%-109% (2.6%-10.2%), and 90.9%-103% (3.0%-9.5%), respectively. EC, 3-MCPD and 2-MCPD were found in some real samples of the soy sauce, wine and flavoring of instant noodle. EC or 3-MCPD was found in some of the salami samples. The method is accurate, fast and suitable for the simultaneous determination of EC, 3-MCPD and 2-MCPD in flavorings.

Key words: chloropropanols, ethyl carbamate, flavorings, gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS), isotope labeled internal standard

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