面粉中脱氧雪腐镰刀菌烯醇标准物质的研制

Development and certification of a reference material for deoxynivalenol in wheat flour

目的目前国内尚缺乏用于质量控制的镰刀菌毒素类生物标准物质,通过研制面粉中脱氧雪腐镰刀菌烯醇化合物的标准物质,期望填补该方面的空缺。方法选择满足JJG 1006—94《一级标准物质》候选物筛选原则和要求的面粉样品作为研制对象,经均质、分装、灭菌后,以同位素稀释-液相色谱-串联质谱法测定脱氧雪腐镰刀菌烯醇含量,经均匀性和稳定性试验后,采用8家实验室联合定值的方法对面粉基质中脱氧雪腐镰刀菌烯醇含量进行定值及不确定度分析。结果随机抽取16袋样品作均匀性检验,分析结果经F检验,统计量F<F_((α=0.05))的临界值,样品均匀性良好。在室温25℃放置一年、44℃放置14天后分别进行了检测,考察其稳定性,测试结果显示特征值在考察时间范围内无明显变化。采用同位素稀释-液相色谱-串联质谱法,与国内8家权威机构实验室进行协同定值,研制得到脱氧雪腐镰刀菌烯醇特征值为(2 366±187)μg/kg。结论本研究提出了面粉中脱氧雪腐镰刀菌烯醇标准物质的研制,为镰刀菌毒素类化合物检测提供质控参考和能力评价依据。

Objective Because of lacking of domestic fusarium mycotoxins reference materials for quality control,the certified reference materials（ CRM） of deoxynivalenol was prepared and certificated.Methods According to the requirements of JJG 1006-94,the wheat flour samples were homogenized,packed and sterilized.Homogeneity,stability studies and assignment of the certified mass fraction were based upon an in-house study using high-performance liquid chromatography isotope-dilution tandem mass spectrometry.Simultaneously,an inter-laboratory comparison study involving eight laboratories was conducted in order to support the in-house certification study.Results Three samples from 16 randomly selected packages were quantitatively analyzed.Shelf life at a storage temperature of 25 ℃ for one year（ longterm stability） or 44 ℃ for 14 days（ short-term stability） was considered.The data were evaluated by ANOVA test.There was no significance of homogeneity and stability.The certified values and the corresponding uncertainty was（2 366 ± 187）μg/kg.Conclusion The natural reference material was produced with a certified deoxynivalenol in wheat flour showing relevant mass fractions.The intended purpose of this reference material,for deoxynivalenol,is not only attributed to laboratory internal quality control but also in facilitating the validation of new analytical methods.