黄瓜中毒死蜱残留基体标准物质的研制

Preparation of matrix reference material for chlorpyrifos residues in cucumber

中文关键词:  标准物质  黄瓜  毒死蜱  定值  不确定度

英文关键词:reference material  cucumber  chlorpyrifos  certificationl  uncertainty

中文摘要:

      目的 建立黄瓜中毒死蜱残留基体标准物质的研制方法。方法 选择符合标准物质研制要求的新鲜黄瓜为研制对象, 经过预冻干、添加、混匀、二次冻干、过筛、包装及辐照灭菌, 采用气相色谱-串联质谱法测定, 同位素内标法定量, 经均匀性和稳定性检验后, 采取多家实验室合作定值的方式进行定值。结果 通过11家独立实验室合作定值及不确定度评估, 毒死蜱的特性值为(0.403±0.033) mg/kg(k=2)。结论 获得的样品均匀性和稳定性良好, 适用于黄瓜中毒死蜱检测过程的方法研制和质量控制。

英文摘要:

      Objective To establish a method for the preparation of chlorpyrifos residues in cucumber. Methods Fresh cucumber which meets the requirements of reference material development was selected as the research object, after pre freeze-drying, adding, mixing, secondary freeze-drying, screening, packaging and irradiation sterilization, the cucumber was determined by gas chromatography tandem mass spectrometry (GC-MS/MS) and quantified by isotope internal standard method. After homogeneity and stability test, the value was determined by cooperation of several laboratories. Results The property value and expanded uncertainty of chlorpyrifos was (0.403±0.033) mg/kg (k=2), certified by 11 independent laboratories. Conclusion The uniformity and stability of the samples are good, which is suitable for the development of the method and quality control of chlorpyrifos poisoning in cucumber.