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QuEChERS-UPLC-MS/MS测定食用菌中四聚乙醛残留及膳食风险评估
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北京市农林科学院

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Determination of metaldehyde residue in edible fungi and dietary risk assessment by QuEChERS-UPLC-MS/MS
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    摘要:

    基于QuEChERS前处理结合超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定食用菌中四聚乙醛残留量的方法,并评估实际样品中的残留状况与膳食风险。样品经乙腈提取,N-丙基乙二胺和十八烷基键合硅胶分散固相萃取净化后,以乙腈-0.1%甲酸水为流动相,经HSS T3色谱柱分离,采用基质匹配曲线内标法定量。结果表明:四聚乙醛在2~200.0 μg/L范围内线性良好(r=0.9998),方法检出限为0.50 μg/kg,方法定量限为1.50 μg/kg。在1.5、15、150 μg/kg添加水平下,平均回收率为72.25%~119.51%,相对标准偏差为0.82%~13.41%。对34份实际样品(大球盖菇、猴头菇、平菇、羊肚菌)检测发现,食用菌样品中四聚乙醛检出率为23.53%,其中羊肚菌中检出率和残留量最高。食用菌样品中慢性与急性膳食摄入风险远低于100%,食品安全指数远小于1,食用菌样品中四聚乙醛的膳食摄入风险均处于可接受范围内。该方法简便、快速、灵敏、重现性好,适用于食用菌中四聚乙醛残留快速精准检测,为食用菌种植中四聚乙醛安全监管和风险评价提供数据支撑。

    Abstract:

    A rapid method was developed for the determination of metaldehyde residues in edible fungi based on QuEChERS pretreatment coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and the residue status and dietary risks in actual samples were evaluated. Samples were extracted with acetonitrile, purified by dispersive solid-phase extraction using primary secondary amine (PSA) and octadecyl-bonded silica (C18), and separated on an HSS T3 column with a mobile phase of acetonitrile-0.1% formic acid in water. Quantification was performed using a matrix-matched internal standard calibration curve. The method showed good linearity for metaldehyde in the range of 2-200.0 μg/L (r = 0.9998). The limit of detection (LOD) and limit of quantification (LOQ) were 0.50 μg/kg and 1.50 μg/kg, respectively. At spiked levels of 1.5, 15, and 150 μg/kg, average recoveries ranged from 72.25% to 119.51%, with relative standard deviations of 0.82%-13.41%. Among 34 actual samples of Stropharia rugosoannulata, Hericium erinaceus, Pleurotus ostreatus, and Morchella spp., the detection rate of metaldehyde was 23.53%, with the highest detection rate and residue level observed in Morchella spp. The chronic and acute dietary exposure risks from these samples were far below 100%, and the food safety index was significantly less than 1, indicating that the dietary intake risks of metaldehyde were all within acceptable limits. This method is simple, rapid, sensitive, and reproducible, making it suitable for accurate detection of metaldehyde residues in edible fungi, and providing data support for safety supervision and risk assessment of its use in mushroom cultivation.

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  • 收稿日期:2026-05-27
  • 最后修改日期:2026-08-19
  • 录用日期:2026-08-19
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