谷物及其制品中脱氧雪腐镰刀烯醇及其衍生物快速检测方法的建立及应用  

Establishment and application of a rapid detection method for deoxynivalenol and its acetylated derivatives in cereal and its products

作　　者：姚远 王兴龙 吕圣吉 薛鸣[1] 任韧[1] 刘少颖[1] YAO Yuan;WANG Xinglong;LYU Shengji;XUE Ming;REN Ren;LIU Shaoying(Hangzhou Center for Disease Control and Prevention,Hangzhou Health Supervision Institution,Hangzhou,Zhejiang 310021,China)

机构地区：[1]杭州市疾病预防控制中心杭州市卫生监督所,浙江杭州310021

出　　处：《中国预防医学杂志》2025年第2期177-185,共9页Chinese Preventive Medicine

基　　金：浙江省医药卫生科技计划项目(2024KY232);中国营养学会科研基金-海普诺凯母婴营养科研专项基金资助项目(CNS-HPNK2021-67);杭州市医药卫生科技项目(A20230034)。

摘　　要：目的建立超高效液相色谱-串联质谱法快速检测谷物及其制品中脱氧雪腐镰刀烯醇(deoxynivalenol,DON)、衍生物3-乙酰脱氧雪腐镰刀烯醇(3-Ac-DON)和15-乙酰脱氧雪腐镰刀烯醇(15-AcDON)的方法,了解DON及衍生物污染状况及暴露风险。方法2022年1月—2023年12月,本研究采集153份谷物及其制品,测定DON及衍生物含量,点评估计算暴露量。根据谷类及其制品基质特点,对仪器分析参数和前处理条件进行优化。样本经50%乙腈水溶液提取稀释,超高效液相色谱-串联质谱仪分离检测,内标法定量。结果DON及其衍生物在5~200μg/L时线性良好,检出限为5~10μg/kg,回收率95.53%~110.76%,相对标准偏差<8.93%。谷物及其制品中DON检出率较高,为75.16%,超标率较低,仅为0.65%。3-Ac-DON和15-Ac-DON污染水平较低,检出率仅为0.65%和6.54%。大部分谷类及其制品主要受DON单一污染,个别玉米类食物存在DON、3-Ac-DON和15-Ac-DON三重污染。不同种类谷类及其制品中DON的污染程度为小麦类>玉米类>大米类,差异有统计学意义(H=77.056,P<0.01)。玉米类三种食物DON污染差异有统计学意义(H=7.287,P<0.05),玉米制品中DON含量低于玉米面,差异有统计学意义(Z=-2.526,P<0.05)。小麦类三种食物差异有统计学意义(H=10.597,P<0.05),方便面中DON的含量高于小麦粉(Z=2.987,P<0.01)和挂面(Z=2.666,P<0.05),差异有统计学意义。居民通过谷物及其制品中DON及衍生物的危害商值分别为27.23%(男性)和33.91%(女性),均<100.00%。结论50%乙腈水溶液提取稀释,超高效液相色谱-串联质谱法简单快捷、灵敏度高,适用于谷类及其制品中DON及其衍生物的测定。通过检测并计算暴露量,风险处于可接受水平。Objective To develop and validate a rapid detection method for the detection of deoxynivalenol(DON)and its derivatives including 3-acetyl-deoxynivalenol(3-Ac-DON)and 15-acetyl-deoxynivalenol(15-Ac-DON)in cereal and its products using ultra-high performance liquid chromatography tandem with mass spectrometry(UPLC-MS/MS),and to assess the contamination status and exposure risk of DON and its derivatives.Methods A total of 153 cereal and its product samples were collected,and the contents of DON and its derivatives were determined to evaluate the exposure levels.Based on the characteristics of cereal and its product matrices,the instrumental analysis parameters and sample pre-treatment conditions were optimized.Samples were extracted and diluted with a 50%acetonitrile-water solution,followed by separation and detection using UHPLC-MS/MS,with quantification performed via the internal standard method.Results A good linearity was observed for DON and its derivatives in the range of 5-200μg/L,with detection limits between 5 and 10μg/kg.The recoveries ranged from 95.53%to 110.76%,with RSDs less than 8.93%.The detection rate of DON in cereal and its products was high at 75.16%,with a low exceedance rate of only 0.65%.The contamination levels of 3-Ac-DON and 15-Ac-DON were relatively low,with detection rates of 0.65%and 6.54%,respectively.Most of the cereal and its product samples were primarily contaminated by DON alone,while a few maize-based foods were contaminated by DON,3-Ac-DON,and 15-Ac-DON.The contamination levels of DON varied among different types of cereal and its products,with wheat-based products>maize-based products>rice-based products(H=77.056,P<0.01).The differences in DON contamination among the three types of corn-based foods are statistically significant(H=7.287,P<0.05).The DON content in corn products is lower than that in corn flour,and the difference is statistically significant(Z=-2.526,P<0.05).The differences among the three types of wheat-based foods are also statistically significant(H=10.597,P<

关 键 词：谷物 脱氧雪腐镰刀菌烯醇 衍生物 污染状况 暴露评估 超高效液相色谱-串联质谱 

分 类 号：TS210.7[轻工技术与工程—粮食、油脂及植物蛋白工程]