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食品研究与开发:2020,41(20):198-203
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快速水蒸气蒸馏-气相色谱热能分析仪法测定肉制品和水产制品中13种N-亚硝胺
(1.天津海关动植物与食品检测中心,天津300461;2.上海海关,上海200002;3.天津海关工业产品安全技术中心,天津300461;4.天津大学精密仪器与光电子工程学院,天津300072)
Determination of 13 N-Nitrosamines in Meat and Aquatic Products by Gas Chromatography-Thermal Energy Analyzer with Rapid Steam Distillation
(1.Animal&Plant and Foodstuffs Inspection Center,Tianjin Customs,Tianjin 300461,China;2.Shanghai Customs,Shanghai 200002,China;3.Technical Center for Safety of Industrial Products,Tianjin Customs,Tianjin 300461,China;4.College of Precision Instrument and Opto-Electronics Engineering,Tianjin University,Tianjin 300072,China)
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投稿时间:2019-11-20    
中文摘要: 建立快速水蒸气蒸馏结合气相色谱-热能分析仪技术测定肉制品和水产制品中13种N-亚硝胺化合物的方法。快速水蒸气蒸馏仪能以较高效率提取样品中亚硝胺类化合物,采用N-亚硝基二异丙胺作为内标可有效提高方法稳定性和回收率。结果表明:在0~1.00 μg/mL质量浓度范围内,13种N-亚硝胺标准曲线线性良好,线性相关系数均可达0.995以上,当取样量为200 g,浓缩体积为1.0 mL时,13种亚硝胺方法检出限为0.05 μg/kg~0.18 μg/kg,定量限为0.17 μg/kg~0.59 μg/kg,添加回收率为80.1%~112.9%,相对标准偏差为1.88%~7.16%。将该方法应用于16个实际样品检测,发现水产制品类样品中N-二甲基亚硝胺检出较多,部分样品含量超过国家限量标准,其他N-亚硝胺化合物偶有检出,含量相对较低。
Abstract:A method for the determination of 13 N-nitrosamines in meat and aquatic products by gas chromatography-thermal energy analyzer with rapid steam distillation was established.The rapid steam distillation apparatus could extract the nitrosamines from samples with high efficiency.The stability and recovery of the method could be effectively improved by using N-nitrodiisopropylamine as internal standard.The results showed that the calibration curves had good linearity in the mass concentration range of 0-1.00 μg/mL with the correlation coefficients greater than 0.995.When the sampling amount was 200 g and the concentration volume was 1.0 mL,the detection limits of 13 nitrosamines were 0.05 μg/kg-0.18 μg/kg,the quantitative limits were 0.17 μg/kg-0.59 μg/kg,the recoveries were 80.1%-112.9%,and the relative standard deviations were 1.88%-7.16%.This method was applied to the detection of 16 real samples.It was found that N-dimethylnitrosamine was more detected in aquatic products,some of the samples even exceeded the national limit standard,and other N-nitrosamines were occasionally detected with relatively low content.
文章编号:202020033     中图分类号:    文献标志码:
基金项目:海关总署科技计划项目(2018IK003)
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