[关键词]
[摘要]
建立基于UPLC-MS/MS测定龙眼及其制品中44种真菌毒素的高通量检测方法。样品经80%乙腈水溶液(V/V,含1%乙酸)提取,PSA和C18净化。采用Waters ACQUITY UPLC BEH C18色谱柱分离,以φ=0.2%甲酸(Formic Acid, FA)-乙腈和水-乙腈为流动相进行梯度洗脱,在正负离子多反应监测模式下内标法定量。结果表明,44种真菌毒素线性关系均良好,R2≥0.990 41,检出限为0.003~0.7 μg/kg,定量限为0.01~2.0 μg/kg;方法的精密度RSD(n=6)为0.7%~9.7%,低、中、高3个添加水平的回收率为70.7%~123.6%。通过对市售17批次龙眼及其制品中44 种真菌毒素进行检测,阳性率为100%,其中15-ADON、Fus X、PAT、TeA等含量较高,说明在龙眼生长、贮藏及加工过程中,这4类真菌毒素为主要污染毒素。采用风险商(Hazard Quotient, HQ)进行膳食暴露风险评估,评估结果显示,21种真菌毒素的风险商值HQ为0~0.012 37,均低于1,说明没有风险,对人体健康威胁性较小。
[Key word]
[Abstract]
A high-throughput method based on UPLC-MS/MS was developed for the determination of 44 mycotoxins in longan and its products. The samples were extracted with 80% acetonitrile-water (V/V) solution containing 1% acetic acid, and purified by PSA and C18. A Waters ACQUITY UPLC BEH C18 column was used for separation, with 0.2% FAacetonitrile and water-acetonitrile as the mobile phase for gradient elution. Quantification was performed using the internal standard method under MRM mode with positive and negative electropry ionization. Results showed that a good linear relationship was found for the 44 mycotoxins, with the correlation coefficients ≥ 0.990 41, the limit of detection ranging within 0.003~0.7 μg/kg, and the limit of quantification being 0.01~2.0 μg/kg. The relative standard deviation (RSD) was 0.7%~9.7% (n=6), and the recoveries of the 44 mycotoxins at three spiking levels (low, intermediate and high levels) ranging within 70.7%~123.6%. The analyses of the 17 batches of longan and its products purchased from market revealed that the positive rate was 100%, with the concentrations of mycotoxins like 15-ADON, Fus X, PAT, TeA were relatively higher, indicating that they were the main contaminated mycotoxins during the growth, storage and processing processes of longan. Hazard Quotient (HQ) was used to assess the dietary exposure risk The assessment results showed that the HQ values of 21 mycotoxins were 0~0.012 37, which were all lower than 1, indicating no risk and little threat to human health.
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[基金项目]
国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(ZZ-2022003;ZZ-2023008);国家市场监督管理总局科技计划项目(2022MK104);海南省重点研发计划项目(ZDYF2023XDNY082)