色谱

色谱

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特丁基二甲基硅烷衍生化气相色谱-质谱联用法快速测定苹果汁中的棒曲霉素

李锋格1*, 姚伟琴1, 田延河1, 李学文2, 张洪霞2, 窦辉1, 朱慧萍1   

  1. 1. 新疆出入境检验检疫局技术中心, 新疆 乌鲁木齐 830063; 2. 新疆农业大学食品科学学院, 新疆 乌鲁木齐 830063
  • 收稿日期:2010-02-18 修回日期:2010-04-18 出版日期:2010-07-28 发布日期:1980-03-25
  • 通讯作者: 李锋格

Rapid determination of patulin in apple juice by tert-butyldimethylsilyl derivatization-gas chromatography-mass spectrometry

LI Fengge1*, YAO Weiqin1, TIAN Yanhe1, LI Xuewen2, ZHANG Hongxia2, DOU Hui1, ZHU Huiping1   

  1. 1. Technical Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China; 2. Food Science Institute, Xinjiang Agriculture University, Urumqi 830063, China
  • Received:2010-02-18 Revised:2010-04-18 Online:2010-07-28 Published:1980-03-25
  • Contact: LI Fengge

PDF

473

被引次数

22

摘要： 运用特丁基二甲基硅烷(TBDMS)衍生化气相色谱-质谱(GC-MS)联用法快速、高灵敏地测定了苹果汁中的棒曲霉素(PAT)。样品用乙酸乙酯-正己烷提取,Carb/C18混合型固相萃取柱净化,TBDMS衍生,GC-MS测定,选择离子监测(SIM)模式,外标法定量。在0.01～1 mg/L的范围内线性良好(r＞0.98),在2～50 μg/kg的添加水平范围内,平均回收率为88%～98%,相对标准偏差(RSD)为5.3%～13.6%, PAT的检出限为0.5 μg/kg,测定低限为2 μg/kg。该方法快速、高灵敏、准确、专一、耐用,适合对苹果汁中PAT进行确证和定量测定。

关键词: 棒曲霉素 , 苹果汁, 气相色谱-质谱, 特丁基二甲基硅烷

Abstract: A gas chromatography-mass spectrometry (GC-MS) method for the quantitative determination and confirmation of patulin in apple juice by tert-butyldimethylsilyl (TBDMS) derivatization was established. The sample was extracted with ethyl acetate-hexane and an aliquot of the supernatant was cleaned up using mixed-mode solid phase extraction (SPE) cartridge containing C18 and graphitized carbon black (GCB), evaporated to dryness under nitrogen gas and the residue was converted to tert-butyldimethylsilyl derivative which was determined with GC-MS in selected ion monitoring (SIM) mode and external standard method was used for quantitative determination. The linear range was from 0.01 to 1 mg/L. The average recoveries were 88%~98% and relative standard deviations were 5.3%~13.6% in the spiked range of 2~50 μg/kg. The limit of detection was 0.5 μg/kg and the limit of quantification and confirmation was 2 μg/kg. The method is rapid, highly sensitive, accurate, specific, rugged and suitable for the quantitative determination and confirmation of patulin in apple juice.

Key words: apple juice, patulin , tert-butyldimethylsilyl (TBDMS), gas chromatography-mass spectrometry (GC-MS)