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

中文关键词:  韭菜冻干粉  腐霉利  标准物质  均匀性  稳定性  同位素稀释

英文关键词:lyophilized Chinese chives  procymidone  certified reference material  homogeneity  Stability  Isotope dilution

中文摘要:

      目的 研制韭菜粉中腐霉利标准物质，联合多家实验室以同位素稀释内标法测试定值。方法 以阳性韭菜为原材料，经过冲洗除杂后，粉碎、添加防腐剂等均质匀浆后冷冻干燥、过筛后混匀，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，60Co-γ射线辐照灭菌等工艺研制韭菜粉中腐霉利标准物质。多家实验室前处理依据标准GB 23200.113-2018《植物源性食品中208种农药及其代谢物残留量的测定气相色谱 质谱联用法》操作，采用同位素稀释内标-气相色谱-串联质谱法进行联合定值。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0.223mg/kg，扩展不确定度为0.021 mg/kg（k=2），在-18℃下冰冻保存有效期达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用质控样品，对于农药腐霉利的精准检测具有重要意义，并可推广应用于快检产品评价、能力验证考核、方法验证等各个领域。

英文摘要:

      Objective To discover a method of the CRM of procymidone in Chinese chives and determine by isotope dilution internal standard.（Methods).It used positive chives as the raw material.after washing and removing impurities, crushing, adding preservatives and homogenized,then freeze-drying, sieving and blending.The CRM of procymidone in Chinese chive powder was prepared under clean and dry conditions by vacuum encapsulation of PE plastic bag with aluminum-plastic composite bag, and 60Coγ-ray irradiation sterilization. Several pretreatments were performed according to standard GB 23200.113-2018, and the value was determined by isotope dilution internal standard-gas chromatography-tandem mass spectrometry. Results: the recovery rate of procymidone was 88.1% ~104.5% , the homogeneity and stability were good, the value was 0.223 mg/kg, the expanded uncertainty was 0.021 mg/kg (K=2) , Tts validity was up to 18 months at-18°C conclusion.It can be used as aquality control sample for the determination of procymidone pesticide residues in laboratory, and it can be popularized and applied in the fields of product evaluation, capability verification, method verification etc..