伏马毒素B_(1)纯度标准物质的研制  

Development of a Certified Reference Material for Fumonisin B_(1)Purity

作　　者：郭文博[1,2] 孟佳佳 牛雪珂 王欣艺 聂冬霞 赵志辉[1] 韩铮[1] GUO Wenbo;MENG Jiajia;NIU Xueke;WANG Xinyi;NIE Dongxia;ZHAO Zhihui;HAN Zheng(Shanghai Academy of Agricultural Sciences,Shanghai 201403,China;Shanghai Kelite Agricultural Product Testing Technology Service Co.,Ltd.,Shanghai 201403,China)

机构地区：[1]上海市农业科学院,上海201403 [2]上海科立特农产品检测技术服务有限公司,上海201403

出　　处：《计量科学与技术》2023年第10期46-53,共8页Metrology Science and Technology

基　　金：上海市科技兴农技术创新项目(沪农科创字(2012)第3-2号);上海市“科技创新行动计划”启明星项目(21QB1403300)。

摘　　要：为更好的满足农产品质量安全检测需求,保证检测结果的准确性、可靠性和可溯源性,研制了伏马毒素B_(1)(FB_(1))纯度标准物质。以实验室自主分离纯化获得的FB_(1)为候选物,通过质谱、红外光谱、核磁共振谱等对其进行定性鉴定。采用质量平衡法和定量核磁法两种不同原理的方法对候选物的纯度进行定值,其中质量平衡法中采用面积归一化法、卡尔费休法、气相色谱串联质谱法和电感耦合等离子体质谱法,分别对候选物中主成分(FB_(1))、水分、挥发性杂质和非挥发性杂质含量进行测定。此外,开展了均匀性检验、稳定性考察,并对研制过程中产生的不确定度进行了系统的评定。结果表明:FB_(1)纯度标准物质量值为99.1%,扩展不确定度为0.3%(k=2),均匀性良好,且满足12个月的稳定性要求。研制的FB_(1)纯度标准物质获得国家二级标准物质证书,编号为GBW(E)100550,能够用于农产品中FB_(1)的定性和定量检测、方法评价以及FB_(1)量值溯源体系的建立。To enhance the accuracy,reliability,and traceability of agricultural product quality safety testing,a certified reference material(CRM)for fumonisin B_(1)(FB_(1))purity was developed.The CRM candidate,obtained through laboratory purification of FB_(1),was qualitatively identified using mass spectrometry,infrared spectroscopy,and nuclear magnetic resonance spectroscopy.The purity of the candidate was quantified using both mass balance and quantitative nuclear magnetic resonance methods.The mass balance method included area normalization,the Karl Fischer method,gas chromatography-tandem mass spectrometry,and inductively coupled plasma mass spectrometry to determine the main component,moisture,volatile and non-volatile impurity contents.Furthermore,homogeneity tests and stability studies were conducted,along with systematic uncertainty evaluations.The results indicated that the FB_(1)CRM has a purity value of 99.1%with an extended uncertainty of 0.3%(k=2),exhibiting good homogeneity and fulfilling a 12-month stability requirement.The developed FB_(1)CRM,certified as a national secondary standard material(GBW(E)100550),is suitable for qualitative and quantitative detection,method evaluation,and establishing a traceability system for FB_(1)in agricultural products.

关 键 词：计量学 伏马毒素B_(1) 纯度标准物质 质量平衡法 定量核磁法 不确定度评定 

分 类 号：TB99[一般工业技术—计量学]