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
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。
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.
标题：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
英文标题：Rapid determination of deoxynivalenol in biscuit by QuEChERS coupled with isotope dilution internal standard-liquid chromatography-tandem mass spectrometry
作者：
吴丹虹 绿城农科检测技术有限公司
周敏 绿城农科检测技术有限公司
周婷婷 绿城农科检测技术有限公司
王川丕 绿城农科检测技术有限公司
黄荣博 绿城农科检测技术有限公司
钟寒辉 绿城农科检测技术有限公司
郭利攀 绿城农科检测技术有限公司
赵月钧 绿城农科检测技术有限公司
孙文闪 绿城农科检测技术有限公司
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,
发表日期：2020-04-24
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