减肥茶中多种真菌毒素的在线免疫亲和净化液相色谱-串联质谱测定研究

    葛宝坤，赵孔祥，陈旭艳

    天津出入境检验检疫局动植食检测中心，天津 300461

    摘要：目的建立在线免疫亲和柱净化-液相色谱-串联质谱快速测定减肥茶中的多种真菌毒素的方法。方法采用PBS/甲醇溶液提取样品中的真菌毒素，再利用可重复使用多功能免疫亲和柱在线净化样品，净化液在线进行液相色谱-串联质谱的测定。结果方法可同时测定减肥茶中伏马毒素、T-2毒素、HT-2毒素、赭曲霉毒素A（OTA）、玉米赤霉烯酮等10种真菌毒素，其最小检出浓度（LOQ）为1～5μg/kg；三水平添加回收率（n=6）为65.3%～102.4%；相对标准偏差（RSD）为4.5%～13.2%。结论本方法在线免疫亲和净化技术与质谱定性定量同时完成，方法简便、快速，检测限满足了国内外减肥茶中真菌毒素限量要求，可用于减肥茶中真菌毒素的快速检测。

   关键词:在线免疫亲和净化；减肥茶；液相色谱-串联质谱；真菌毒素；伏马毒素；T-2毒素；HT-2毒素；赭曲霉毒素A；玉米赤霉烯酮

    中图分类号：R155.5　文献标识码：B

    Determination of mycotoxins in slimming teaby on-line

    immunoaffinity column coupled HPLC-MS/MS

    GE Bao-kun, ZHAO Kong-xiang, CHEN Xu-yan

    Tianjin Entry-exit Inspection and QuarantineBureau, Tianjin 300461,China

    Abstract:   Objective  To establish a method based on reusable on-line immunoaffinitypurification coupled with HPLC-MS/MS, and to analyze 10 kinds ofmycotoxins including fumonisins, T-2, HT-2, Ochratoxin (OTA),zearalenone, zearalanone, α-zearalanol, β-zearalanol, α-zearalenoland β-zearalenol in slimming tea.  Methods   Thetarget compounds were extracted by phosphate buffered saline (PBS)/methanol, the sample purification was completed by the on-lineimmunoaffinity column before detection by HPLC-MS/MS.  Results    The limits of quantification (LOQ) were1~5μg/kg. Recovery studies were performed at three fortificationlevels (n=6). The recovery rat was 65.3%~102.4% with the relativestandard deviation of 4.5%~13.2%.  Conclusion    The immunoaffinity purification anddetection by mass detector are completed simultaneously. The methodis time-effective and cost-effective, and could be applied forseparating and quantifying mycotoxins in slimming tea.

    Key words:   On-line immunoaffinitypurification; Slimming tea; HPLC-MS/MS; Mycotoxins; Fumonisins; T-2toxin; HT-2 toxin; Ochratoxin; Zearalenone

    《中国国境卫生检疫杂志》