QuEChERS-同位素稀释内标法-液相色谱-串联质谱法快速测定饼干中的脱氧雪腐镰刀菌烯醇

Rapid determination of deoxynivalenol in biscuit by QuEChERS coupled with isotope dilution internal standard-liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  同位素稀释内标法  液相色谱-串联质谱法  饼干  脱氧雪腐镰刀菌烯醇

英文关键词:QuEChERS  isotope dilution internal standard  liquid chromatography-tandem mass  biscuit  deoxynivalenol

中文摘要:

      目的 建立QuEChERS-同位素稀释内标法-液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速测定饼干中的脱氧雪腐镰刀菌烯醇。方法 样品加入13C15-脱氧雪腐镰刀菌烯醇同位素内标后, 用水-乙腈(4/1, V/V)溶液提取、旋涡超声离心后, 取上清液2.0 mL经N-丙基乙二胺(primary secondary amine, PSA)吸附剂、C18吸附剂净化, 净化液过滤膜, 采用LC-MS/MS进行测定。结果 在优化的实验条件下, 脱氧雪腐镰刀菌烯醇的检出限为0.6 μg/kg, 定量限为2.0 μg/kg。在线性范围0.4~50.0 μg/L内, 相关系数为0.9995。平均加标回收率为82.1%～92.3%, 相对标准偏差4.3%~6.6%(n=6)。结论 该方法简单、快速, 可用于饼干中的脱氧雪腐镰刀菌烯醇的快速测定。

英文摘要:

      Objective To establish a method for the rapid determination of the deoxynivalenol (DON) in biscuit by QuEChERS and isotope dilution internal standard method coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods After adding isotope internal standard, the sample was extracted with water and acetonitrile solution (4/1, V/V). After vortex and ultrasound centrifugation, 2.0 mL supernatant was purified by N-primary secondary amine, (PSA) and C18, and then was filtrated by filtration membrane and determinated by LC-MS/MS. Results Under the optimized experimental conditions, the detection limit of DON was 0.6 μg/kg, and the limits of quantitation was 2.0 μg/kg. In the linear range of 0.4–50.0 μg/L, the correlation coefficient was 0.9995. The average recovery was 82.1%–92.3%, and the relative standard deviation (RSD) was 4.3%–6.6% (n=6). Conclusion This method is simple, accurate and reliable, which can be used for the rapid detection of DON in biscuit.