首页|龙眼及其制品中44种真菌毒素高通量检测方法的建立及其膳食暴露风险评估

龙眼及其制品中44种真菌毒素高通量检测方法的建立及其膳食暴露风险评估

Development of a High-throughput Detection Assay and Dietary Exposure Risk Assessment for 44 Mycotoxins in Longan and Its Products

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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.
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%FA-acetonitrile 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.

UPLC-MS/MSmycotoxinsdetectiondietary exposure risk assessment

尹青春、陈小妹、周凌聿、陈春泉、高云慨、李备、梁成美、邓英林、邓浩

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海南省检验检测研究院食品检验检测中心,国家市场监管重点实验室(热带果蔬质量与安全),海南海口 570314

海南医学院热带医学院环境科学系,海南海口 570000

海南省农业科学院农产品加工设计研究所,海南省热带果蔬冷链研究重点实验室,海南海口 571100

超高效液相色谱-串联质谱 真菌毒素 检测 膳食暴露风险评估

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)自主研究课题国家市场监督管理总局科技计划项目海南省重点研发计划项目

ZZ-2022003ZZ-20230082022MK104ZDYF2023XDNY082

2024

现代食品科技
华南理工大学

现代食品科技

CSTPCD北大核心
影响因子:1.07
ISSN:1673-9078
年,卷(期):2024.40(7)