氣相色譜法測定魚肉中指示性多氯聯苯的不確定度評定
Uncertainty Evaluation of Indicative Polychlorinated Biphenyls in Fish by Gas Chromatography
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摘要: 為了提高實驗室檢測結果的準確性,對氣相色譜法測定魚肉中指示性多氯聯苯含量進行了不確定度的評定。依據食品安全國家標準GB 2762-2022《食品安全國家標準食品中污染物限量》,識別“被測量”為樣品中“以2,4,4’-三氯聯苯( PCB 28) 、2,2’,5,5’-四氯聯苯(PCB52)、2,2’,4,5,5’-五氯聯苯(PCB101)、2, 3’,4,4’,5-五氯聯苯(PCB118)、2,2’,3,4,4’,5’-六氯聯苯(PCB138)、2,2’,4,4’,5,5’-六氯聯苯(PCB153)和 2,2’,3,4,4’,5,5’-七氯聯苯(PCB180)總和計”的多氯聯苯含量,根據“被測量”及檢測標準,重新建立多氯聯苯測量模型,分析測量模型中對結果有影響的不確定度分量,并進行評定。經評定,質控魚肉樣品中多氯聯苯的測量結果為149.1 μg/kg,相對擴展不確定度Ur=2.9%,k=2。不確定度貢獻為:測量重復性70.8%、稱樣質量0.025%、加入內標體積1.8%、樣品溶液中各目標物濃度比值之和27.3%。Abstract: In order to ensure the accuracy of laboratory test results, the uncertainty of the determination of indicative polychlorinated biphenyls in fish by gas chromatography was evaluated. According to the national Food Safety standard, National Food Safety Standard Maximum Levels of Contaminants in Foods (GB 2762-2022), the content of PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in the "measured" samples was determined as the total content of PCBs. Then, the polychlorinated biphenyls (PCBs) measurement model was re-established according to the "measured" and detection standard, and then the weight of uncertainty affected by the measurement model on test results were analyzed and evaluated. After evaluation, the measurement result of PCBs in quality control fish samples was 149.1 μg/kg, and the relative extended uncertainty was Ur=2.9%, k=2. The contribution of uncertainty was measurement repeatability 70.8%, sample weight 0.025%, internal standard volume 1.8%, sum of concentration ratios of each target in sample solution 27.3%.