QuEChERS-超高效液相色谱-串联质谱法测定花生及土榨花生油中9种真菌毒素

Determination of 9 kinds of mycotoxins in peanuts and flavor peanut oil by QuEChERS-ultra performance liquid chromatography- tandem mass spectrometry

中文关键词:  QuEChERS  超高效液相色谱-串联质谱法  土榨花生油  真菌毒素  超高比表面积单壁碳纳米管

英文关键词:QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  flavor peanut oil  mycotoxins  ultra-high surface area single-walled carbon nanotubes

中文摘要:

      目的 建立QuEChERS净化-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定花生及土榨花生油中9种真菌毒素的分析方法。方法 样品经1%甲酸甲醇溶液提取, 用QuEChERS分散吸附剂净化除杂, 以0.1%甲酸水溶液和乙腈为流动相梯度洗脱, 经ACE Excel 3 C18色谱柱(2.1 mm×100 mm, 3 μm)分离, 在电喷雾(electrospray ionization, ESI)正负离子切换扫描模式下, 采用多反应监测(multiple reaction monitoring, MRM)进行分析, 外标法进行定量。 结果 9种真菌毒素在0.5~50 μg/L的浓度范围内线性关系良好, 相关系数(r2)≥0.9937, 检出限和定量限分别为0.03~1.14 μg/kg和0.10~3.50 μg/kg。在低、中、高3个添加水平(2、10、20 μg/kg)下的回收率为73.1%~117.7%, 相对标准偏差范围为0.6%~6.5%之间(n=6)。结论 本方法操作简单、灵敏度高、适用性强, 适用于花生及土榨花生油等9种真菌毒素的快速筛查及定量检测。

英文摘要:

      Objective To establish a method for the determination of 9 kinds of mycotoxins in peanuts and flavor peanut oil by QuEChERS extraction technology and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted with 1% formic acid methanol solution, purified with QuEChERS dispersed adsorbent, eluted with 0.1 % formic acid aqueous solution and acetonitrile as mobile phase, and separated by ACE Excel 3 C18 column (2.1 mm×100 mm, 3 μm). In the electrospray ionization (ESI) positive and negative ion switching scanning mode, the samples were analyzed by multi-reaction monitoring multiple reaction monitoring (MRM) and quantified by external standard method. Results Nine kinds of mycotoxins had good linear relationships in the concentration range of 0.5?50 μg/L, the correlation coefficient (r2)≥0.9937, the detection limits and quantitative limits were 0.03?1.14 μg/kg and 0.10?3.50 μg/kg, respectively. The recoveries at low, medium and high addition levels (2, 10, 20 μg/kg) were 73.1%?117.7%, and the relative standard deviation were 0.6%?6.5% (n=6). Conclusion This method has the advantages of simple operation, high sensitivity and strong applicability, and is suitable for rapid screening and quantitative detection of 9 kinds of mycotoxins such as peanut and flavor peanut oil.