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

Determination of mycotoxins in slimming tea by on-line immunoaffinity column coupled HPLC-MS/MS

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。

Objective To establish a method based on reusable on-line immunoaffinity purification coupled with HPLC-MS/MS, and to analyze 10 kinds of mycotoxins including fumonisins, T-2, HT-2, Ochratoxin （OTA）, zearalenone, zearalanone, α-zearalanol, β-zearalanol, α-zearalenol and β-zearalenol in slimming tea. Methods The target compounds were extracted by phosphate buffered saline （PBS）/methanol, the sample purification was completed by the on-line immunoaffinity column before detection by HPLC-MS/MS. Results The limits of quantification （LOQ） were 1- 5μg/kg. Recovery studies were performed at three fortification levels （n=6）. The recovery rat was 65.3%-102.4% with the relative standard deviation of 4.5%-13.2%. Conclusion The immunoaffinity purification and detection by mass detector are completed simultaneously. The method is time-effective and cost-effective, and could be applied for separating and quantifying mycotoxins in slimming tea.