韭菜粉中腐霉利标准物质的研制

Preparation of certified reference material of procymidone in Allium tuberosum powder

目的研制韭菜粉中腐霉利标准物质,并联合多家实验室以同位素稀释内标法测试定值。方法以含腐霉利的韭菜为原材料,样品经冲洗除杂、粉碎、添加防腐剂、均质、匀浆、冷冻干燥后,过筛混匀,在洁净干燥条件下以聚乙烯塑料袋外套铝塑复合袋真空封装,再由^(60)Co-γ射线辐照灭菌,最终研制出韭菜粉中腐霉利标准物质。依据GB 23200.113—2018《食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定》中气相色谱-质谱法的前处理方法,多家实验室采用同位素稀释内标-气相色谱-串联质谱法对腐霉利的含量进行联合定值。结果韭菜粉中腐霉利标准物质回收率为88.1%~104.5%,均匀性和稳定性良好,特性值为0.223 mg/kg,扩展不确定度为0.021 mg/kg(k=2),在–18℃下冰冻保存有效期为18个月。结论所制备的韭菜粉中腐霉利标准物质可作为实验室腐霉利农药残留检测的质控样品,对于农药腐霉利的精准检测具有重要意义,可推广应用于快速检测产品评价、能力验证考核、方法验证等各个领域。

Objective To prepare the standard substances of procymidone in Allium tuberosum and determine the value by isotope dilution internal standard method in collaboration with several laboratories.Methods Used Allium tuberosum containing procymidone as raw material,the samples were rinsed and cleaned,crushed,added preservatives,homogenized,homogenized,freeze-dried,screened and mixed,vacuum-packaged in polyethylene plastic bag with aluminum-plastic composite bag under clean and dry conditions,and then sterilized by ^(60)Co-γ-ray irradiation.Finally,the standard material of procymidone in Allium tuberosum powder was prepared.Accorded to the pre-treatment method of gas chromatogram-mass spectrometry in GB 23200.113—2018 National standard for food safety-Determination of residues of 208 kinds of pesticides and their metabolites in plant origin foods,multiple laboratories used isotope dilution internal standard-gas chromatography tandem mass spectrometry to jointly determine the content of prochlorperazine.Results The recoveries of the standard substance of procymidone in Allium tuberosum powder putrescide were 88.1% to 104.5%,with good uniformity and stability.The characteristic value was 0.223 mg/kg,and the expanded uncertainty as 0.021 mg/kg(k=2).The shelf life of frozen storage at -18℃was 18 months.Conclusion The standard material of procymidone in the prepared Allium tuberosum powder can be used as the quality control sample for the detection of pesticide residue of procymidone in the laboratory,which is of great significance for the accurate detection of pesticide procymidone,and can be applied to various fields such as rapid detection product evaluation,capability verification and method verification.