辣椒油中苯并芘参考标准物质的制备与定值

为建立辣椒油中苯并芘标准物质的研制和定值方法，向辣椒油中添加一定量的苯并芘标准溶液，搅拌均匀后分装100 瓶，随机抽取10 瓶样品进行样品均匀性检验，在95% 置信区间内，检验结果同时通过F 检验和t 检验。在恒温4℃冷藏和常温20℃条件下，在8 周内进行样品的稳定性检验，检验结果通过t 检验，在95% 置信区间内。并通过分析标准物质制备过程中的不确定度来源，计算出不确定度分量、合成标准不确定度及扩展不确定度。制备的辣椒油中苯并芘采用同位素稀释气相色谱- 质谱联用法进行辣椒油中苯并芘定值，定值后的辣椒油样品中苯并芘含量为(9.98 ± 0.914)μg/kg(k ＝ 2)。本标准物质对于植物油中苯并芘检测的方法验证和质量控制具有重要意义。

Preparation,Testing and Certification of Reference Materials for Benzo(a)pyrene in Pepper Oil

A methodology regarding preparation and certification of the reference material for Benzo(a)pyrene in pepper oil was presented. Spiked pepper oil was packed in 100 bottles after homogenization and 10 of these 100 bottles were selected to test the homogeneity of the sample. Two batches of 10 samples from these 100 bottles were kept at 4 ℃ and 20 ℃, respectively. The stabilities of 20 bottles were analyzed e once a week for 8 consecutive weeks. Test results demonstrate the homogeneity and stability of that the pepper oil sample. Benzo(a)pyrene was determined by gas chromatography-mass spectrometry, based on isotope dilution. Uncertainty components, combined standard uncertainty and expanded uncertainty were also calculated, and the concentration of the sample was certified as (9.98 ± 0.914 )μg/kg, k = 2. The reference material is intended for use in the methodological validation and quality control for benzo(a)pyrene in edible vegetable oils