色谱 ›› 2017, Vol. 35 ›› Issue (2): 185-190.DOI: 10.3724/SP.J.1123.2016.07008

• 研究论文 • 上一篇    下一篇

实时直接分析-串联质谱法测定葡萄酒中赭曲霉毒素A

宫小明1, 马荣桧1, 王洪涛1, 郭礼强1, 李凯1, 吴振兴2, 赵晗1, 孙军1   

  1. 1. 潍坊出入境检验检疫局, 山东 潍坊 261041;
    2. 山东出入境检验检疫局检验检疫技术中心, 山东 青岛 266002
  • 收稿日期:2016-07-07 出版日期:2017-02-08 发布日期:2013-06-09
  • 通讯作者: 宫小明,Tel:(0536)8582599,E-mail:salmon_g@hotmail.com
  • 基金资助:

    国家质检总局科研基金资助项目(2013IK177).

Determination of ochratoxin A in wine by direct analysis in real time-tandem mass spectrometry

GONG Xiaoming1, MA Ronghui1, WANG Hongtao1, GUO Liqiang1, LI Kai1, WU Zhenxing2, ZHAO Han1, SUN Jun1   

  1. 1. Weifang Entry-Exit Inspection and Quarantine Bureau, Weifang 261041, China;
    2. Technical Center, Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China
  • Received:2016-07-07 Online:2017-02-08 Published:2013-06-09
  • Supported by:

    Scientific Research Fund Project of General Administration of Quality Supervision and Inspection and Quarantine of the Peoples Republic of China (No. 2013IK177).

摘要:

建立了葡萄酒中赭曲霉毒素A的实时直接分析-串联质谱(DART-MS/MS)方法。前处理采用乙酸乙酯提取,二甲基十八碳硅烷粉(ODS)粉分散固相萃取净化,采用DART-MS/MS检测,同位素稀释内标法定量。结果表明:在1.0、2.0、10 μg/kg3个加标水平下,回收率为88.7%~105.7%,RSD为8.5%~12.8%,定量限为0.5 μg/kg。该方法具有简单、快速、灵敏度高等特点,能满足葡萄酒中赭曲霉毒素A检测的要求。

关键词: QuEChERS, 串联质谱法, 葡萄酒, 实时直接进样分析, 同位素稀释内标, 赭曲霉毒素A

Abstract:

A method for the determination of ochratoxin A (OTA) in wine was developed using direct analysis in real time-electrospray ionization tandem mass spectrometry (DART-MS/MS). The sample was extracted with ethyl acetate and purified by votexing with ODS powder, detected using DART-MS/MS. The results showed that the average recoveries ranged from 88.7% to 105.7% with the RSDs of 8.5%-12.8% at three spiked levels of 1.0, 2.0, and 10 μ g/kg. The LOQ was 0.5 μg/kg. The proposed method was accurate, rapid and reliable, which can be successfully applied to the qualitative and quantitative analysis of ochratoxin A in wine.

Key words: direct analysis in real time (DART), isotope dilution internal standard, ochratoxin A (OTA), QuEChERS, tandem mass spectrometry (MS/MS), wine

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