色谱

色谱 ›› 2012, Vol. 30 ›› Issue (09): 903-907.DOI: 10.3724/SP.J.1123.2012.05007

• 研究论文 • 上一篇    下一篇

超高效液相色谱-电喷雾串联质谱法直接测定黄酒和葡萄酒中氨基甲酸乙酯

王丽娟1, 柯润辉1,2*, 王冰3, 尹建军1,2, 宋全厚1,2   

  1. 1. 中国食品发酵工业研究院, 北京 100027; 2. 国家食品质量监督检验中心, 北京 100027; 3. 沃特世科技(上海)有限公司, 上海 201203
  • 收稿日期:2012-05-07 修回日期:2012-06-05 出版日期:2012-09-28 发布日期:2012-09-20
  • 通讯作者: 柯润辉,博士,高级工程师,主要研究方向为食品安全检测与分析. Tel: (010)64647447, E-mail: kerunhui@yahoo.com.cn.
  • 基金资助:

    中国食品发酵工业研究院科技发展基金(2011KJFZ-BS-01).

Direct determination of ethyl carbamate in Chinese rice wine and grape wine by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry

WANG Lijuan1, KE Runhui1,2*, WANG Bing3, YIN Jianjun1,2, SONG Quanhou1,2   

  1. 1. China National Research Institute of Food & Fermentation Industries, Beijing 100027, China; 2. National Food Quality Supervision and Inspection Center, Beijing 100027, China; 3. Waters Technologies (Shanghai) Limited, Shanghai 201203, China
  • Received:2012-05-07 Revised:2012-06-05 Online:2012-09-28 Published:2012-09-20

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429

被引次数

31

摘要： 建立了超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)直接测定黄酒和葡萄酒中氨基甲酸乙酯含量的方法。黄酒和葡萄酒样品经蒸馏水简单稀释后,过0.22 μm微孔滤膜,直接进行UPLC-MS/MS分析检测。以Waters Acquity UPLCTMBEH C18色谱柱为分析柱,乙腈和0.1%(v/v)乙酸水溶液为流动相,采用电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,以氨基甲酸丁酯(BC)作为内标进行定量。结果表明: 方法在2～500 μg/L的范围内线性关系良好(相关系数大于0.995),其对黄酒和葡萄酒的检出限为1.7 μg/L,定量限为5.0 μg/L,可达到黄酒和葡萄酒中氨基甲酸乙酯的检测要求。当添加水平为10、20和100 μg/L时,黄酒和葡萄酒中待测组分的回收率为90%～102%,日内精密度(n=6)为0.8%～4.5%,日间精密度(n=6)为1.4%～5.6%。该方法样品处理简单,前处理过程不使用有机溶剂,测定快速、准确,灵敏度高,非常适合黄酒和葡萄酒中氨基甲酸乙酯的快速检测和定量分析。

关键词: 氨基甲酸乙酯, 超高效液相色谱, 电喷雾离子化串联质谱, 黄酒, 葡萄酒

Abstract: An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometric (UPLC-ESI-MS/MS) method was established for the direct determination of ethyl carbamate in Chinese rice wine and grape wine. The Chinese rice wine and grape wine samples were diluted with distilled water, filtered through 0.22 μm microporous membrane. The LC separation was performed on a Waters Acquity UPLC system with a BEH C18 column, acetonitrile and 0.1% (v/v) acetic acid aqueous solution as the mobile phase. The ethyl carbamate was determined in the mode of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM). The butyl carbamate (BC) was used as the internal standard for the quantitative determination. The calibration curve showed good linearity in the range of 2~500 μg/L with the correlation coefficient greater than 0.995. The limit of detection (LOD) was 1.7 μg/L and the limit of quantification (LOQ) was 5.0 μg/L. The recoveries of the ethyl carbamate in Chinese rice wine and grape wine was in the range of 90%~102%. The relative standard deviations (RSDs) of intra-day and inter-day determinations were 0.8%~4.5% and 1.4%~5.6% (n=6). The results indicated that the proposed method is easy, fast, sensitive, and suitable for the determination of ethyl carbamate in Chinese rice wine and grape wine.

Key words: Chinese rice wine, electrospray ionization tandem mass spectrometry (ESI-MS/MS), ethyl carbamate, grape wine, ultra performance liquid chromatography (UPLC)