摘要
[目的]本文旨在研制脱氧雪腐镰刀菌烯醇(deoxynivalenol,DON)国家级纯度标准物质,为农产品中DON的检测等工作提供物质基础。[方法]利用质量平衡法和定量核磁共振法对DON纯度标准物质进行纯度定值。质量平衡法包括采用液相色谱面积归一化法测定DON主成分含量,采用卡尔费休库仑法测定纯度标准物质中水分含量,采用顶空气相色谱-质谱法测定挥发性杂质含量,以及采用电感耦合等离子质谱法测定无机离子杂质含量。定量核磁共振法采用苯甲酸为内标,选择合适的共振峰,内标法定量标准物质的纯度,并对标准物质进行均匀性、稳定性检测和不确定度评估。[结果]质量平衡法的纯度定值结果为99.47%,定量核磁共振法定值结果为99.45%,最终所研制的DON纯度标准物质的纯度为99.5%,扩展不确定度为0.4%,均匀性良好,且满足12个月以上的稳定性要求。[结论]本试验所研制的DON纯度标准物质符合国家标准物质技术规范,目前已被批准为国家一级标准物质,并已被用于小麦、玉米等农产品实际检测过程中。
[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.
作者
孟佳佳
郭文博
聂冬霞
韦阳
赵志辉
韩铮
MENG Jiajia;GUO Wenbo;NIE Dongxia;WEI Yang;ZHAO Zhihui;HAN Zheng(Institute for Agro-food Standards and Testing Technology,Shanghai Academy of Agricultural Sciences,Shanghai 201403,China;School of Agriculture and Biology,Shanghai Jiao Tong University,Shanghai 200240,China)
出处
《南京农业大学学报》
CAS
CSCD
北大核心
2024年第3期564-574,共11页
Journal of Nanjing Agricultural University
基金
国家自然科学基金项目(32272442)。
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
deoxynivalenol
reference material
mass balance method
quantitative nuclear magnetic resonance method
evaluation of uncertainty
