超高效液相色谱-串联质谱法检测小麦中19种真菌毒素

Determination of 19 kinds of mycotoxins in wheat by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  小麦  风险评估  高通量  真菌毒素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  wheat  risk assessment  high throughput  mycotoxin

中文摘要:

      目的 建立超高效液相色谱-串联质谱法检测小麦中19种真菌毒素。方法 样品经乙腈-水-乙酸(70:29:1, V:V:V)振荡提取并低温高速离心后, 直接用水稀释提取液并再次低温高速离心, 上清液过膜后经Hypersil Gold C18反相色谱柱(100 mm×2.1 mm, 1.9 μm)分离, 最后用三重四极杆质谱在多反应监测模式下外标法定量测定。结果 在最佳分析条件下, 各真菌毒素靶标线性范围均良好, 相关系数(r2)均大于0.999; 检出限和定量限分别为0.001~5.000 μg/kg和0.003~15.000 μg/kg; 在3个不同浓度下的加标回收率位于77.08%~119.77%之间, 相对标准偏差为0.59%~9.99% (n=6)。结论 该方法操作简单、稳定可靠、检测通量高、检测成本低, 有望用于大批量小麦产品中真菌毒素质量安全风险评估筛查及验证分析, 为政府部门粮食质量安全监管提供技术支撑。

英文摘要:

      Objective To develop a method for the determination of 19 kinds of mycotoxins in wheat by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with acetonitrile-water-acetic acid (70:29:1, V:V:V) shaking and centrifuged at high speed at low temperature, the extract was directly diluted with water and centrifuged again with high speed at low temperature, after the supernatant was passed through the membrane, it was separated on a Hypersil Gold C18 reversed-phase chromatographic column (100 mm× 2.1 mm, 1.9 μm), finally, it was quantified by using a triple quadrupole mass spectrometer in a multi-reaction monitoring mode using an external standard method. Results Under the optimal analytical conditions, the linear ranges of each mycotoxin target were good, and the correlation coefficients (r2) were greater than 0.999; the limits of detection and limits of quantitation were 0.001?5.000 μg/kg and 0.003?15.000 μg/kg, respectively; the recoveries at the 3 different concentrations were within the range of 77.08%?119.77%, and the relative standard deviations were 0.59%?9.99% (n=6). Conclusion This method is simple, stable, reliable, high in detection flux and low in detection cost, it is expected to be used for the risk assessment, screening and verification analysis of mycotoxin quality and safety in large quantities of wheat products, and provide technical support for food quality and safety supervision of government departments.