牛乳中二噁英类化合物标准物质的研制  

Preparation and certification of a reference material on PCDD /Fs and dl-PCBs in milk

作　　者：王向勇[1,2] 张磊 李敬光[1,2] 赵云峰 

机构地区：[1]南昌大学,江西南昌330031 [2]国家食品安全风险评估中心,北京100050

出　　处：《中国食品卫生杂志》2014年第3期205-209,共5页Chinese Journal of Food Hygiene

基　　金："十二五"国家科技支撑计划课题(2011BAK10B07)

摘　　要：目的研制乳粉中非添加二噁英类化合物的标准物质,加强我国二噁英类化合物实验室检测质控能力建设。方法选择满足侯选物筛选原则和要求的牛乳样品作为候选物,经混匀、分装、冻干后,以高分辨气相色谱-高分辨质谱法同位素稀释技术测定多氯代苯并二噁英、多氯代苯并呋喃(PCDD/Fs)和二噁英样多氯联苯(dl-PCBs),经均匀性和稳定性试验后,采用多家实验室联合定值方法对样品中二噁英类化合物含量进行定值及不确定度分析。结果经单因素方差分析和F检验,瓶间均匀性试验的检验值F均小于临界值F0.01(9,40)。室温下1年的稳定性试验结果显示,定值化合物一元线性拟合方程中斜率|b1|均小于t(0.95,3)×s(b1),表明特征值变化趋势无统计学意义。结论本研究提出了二噁英类化合物定值结果,为二噁英检测提供质控参考和能力评价。Objective To enhance the laboratory ability of quality control and method validation in the determination of natural occurring PCDD/Fs, dl-PCBs and their analoguesin milk, thereference material was prepared and certificated. MethodsThe milk samples were homogenized, packed and cryodesiccated, then the PCDD/Fs and dl-PCBs were analyzed by high resolution gas chromatography/high resolution mass spectrometry using isotope dilution and internal standard quantization techniques. Afterthe homogeneity and stabilitytest, the certification was conducted with 5qualified laboratories. ResultsThe 10bottles of milk samples were randomly selected and were tested for the cross-sample homogeneity, and PCDD/Fs and dl-PCBs in milk samples were homogeneous. The stabilities of the PCDD/Fs and dl-PCBs in milk samples were tested over one year at room temperature and the levels were stabilized.ConclusionThe natural reference material of PCDD/Fs and dl-PCBs in milk was first prepared and certificated and was intended to be used for quality control and method validation in the determination of PCDD/Fs, dl-PCBs and their analoguesin milk samples.

关 键 词：乳粉 高分辨气相色谱-高分辨质谱法 二噁英类化合物 标准物质 实验室质量控制 食品安全 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]