南京农业大学学报2024，Vol.47Issue(3)：564-574,11.DOI:10.7685/jnau.202304010
农产品检测用脱氧雪腐镰刀菌烯醇纯度标准物质的研制
Development of deoxynivalenol purity certified reference materials for agricultural products detection
摘要
Abstract
[Objectives]The purpose of this paper was to develop the certified reference material(CRM)of deoxynivalenol(DON),so as to provide materials basis for the requirements of DON detection in agricultural products.[Methods]The purity of the prepared DON CRM was determined by two methods,including mass balance method and quantitative nuclear magnetic resonance(qNMR)method.The mass balance method included the determination of DON principal component content by liquid chromatography-area normalization method,the determination of moisture content in DON purity certified reference material by Karl Fischer Coulomb method,the determination of volatile impurity content by headspace gas chromatography-mass spectrometry(GC-MS),and the determination of inorganic ion impurity content by inductively coupled plasma mass spectrometry(ICP-MS).With regard to qNMR approach,benzoic acid was used as the internal standard,and the purity was accurately quantified by the internal standard method with appropriate resonance peaks.The obtained DON CRM was further verified by determination of the uniformity and stability,and the uncertainties were thoroughly evaluated.[Results]The purities of DON determined by mass balance method and qNMR approach were 99.47%and 99.45%,respectively.The purity of the prepared CRM was assigned as 99.5%with the expanded uncertainty of 0.4%.The homogeneity and the stability for 12 months at storage conditions were satisfactory.[Conclusions]The newly developed CRM in this experiment fulfilled the requirements of the Regulation of Reference Materials.It had been approved as first class of National CRM and had been used in actual DON detection in agricultural products,i.e.,maize and wheat.关键词
脱氧雪腐镰刀菌烯醇/标准物质/质量平衡法/定量核磁共振法/不确定度评估Key words
deoxynivalenol/reference material/mass balance method/quantitative nuclear magnetic resonance method/evaluation of uncertainty分类
化学化工引用本文复制引用
孟佳佳,郭文博,聂冬霞,韦阳,赵志辉,韩铮..农产品检测用脱氧雪腐镰刀菌烯醇纯度标准物质的研制[J].南京农业大学学报,2024,47(3):564-574,11.基金项目
国家自然科学基金项目(32272442) （32272442）
