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建立了蜂王浆冻干粉中甲硝唑残留标准样品的研制和定值方法。对日常检测阳性样品进行匀浆、冷冻干燥和均匀化加工处理,真空包装,得到1批400袋蜂王浆冻干粉样本。F检验法和t检验法表明在95%置信区间内,样本均匀性、短期稳定性和长期稳定性均达到标准样品要求。制备的甲硝唑标准样品采用液相色谱-串联质谱法,与国内外8家实验室进行协同定值。采用格拉布斯和柯克伦检验对定值结果进行异常值检验,并对结果进行不确定度评估。
A standard method for the determination of metronidazole residue in the lyophilized royal jelly powder was established. Positive samples were routinely tested for homogenization, freeze-drying and homogenization processing, and vacuum-packed to obtain 1 batch of 400 bags of lyophilized powder samples of royal jelly. F test and t test showed that the sample uniformity, short-term stability and long-term stability meet the standard sample requirements within a 95% confidence interval. The metronidazole standard sample prepared by liquid chromatography - tandem mass spectrometry, and eight laboratories at home and abroad for collaborative valuation. Grubbs and Kirklean tests were used to test outliers for outliers and the results were evaluated for uncertainty.