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预防医学  2023, Vol. 35 Issue (8): 726-731    DOI: 10.19485/j.cnki.issn2096-5087.2023.08.018
  实验技术 本期目录 | 过刊浏览 | 高级检索 |
即食水产制品N-亚硝胺类化合物检测的样品处理方法优化研究
陈婧, 王立媛, 胡争艳, 汤鋆, 吴平谷
浙江省疾病预防控制中心理化与毒理检验所,浙江 杭州 310051
Optimization of pretreatment methods for N-nitrosamine compounds in ready-to-eat aquatic products
CHEN Jing, WANG Liyuan, HU Zhengyan, TANG Jun, WU Pinggu
Department of Physicochemical and Toxicology, Zhejiang Provincial Center for Disease Control and Prevention, Hangzhou, Zhejiang 310051, China
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摘要 目的 优化即食水产制品中N-亚硝胺类化合物的前处理方法。方法 采集市售即食水产制品样品,均质后经水蒸气蒸馏,取蒸馏液加入乙醇(分散剂)、三氯甲烷(萃取剂)和3.0 g氯化钠进行分散液液微萃取(DLLME),萃取时间为10 min。离心后取下层有机相,采用气相色谱-三重四极杆质谱法(GC-MS/MS)多反应监测模式测定6种N-亚硝胺类化合物,以内标法定量。结果 6种N-亚硝胺类化合物在10.0~500 μg/L线性范围较好,相关系数均>0.999;方法检出限为0.05~0.6 μg/kg,定量限为0.15~1.6 μg/kg;平均加标回收率为71.8%~108.9%,相对标准偏差(RSD)为1.4%~8.6%。检测市售即食水产制品样品20份,N-二甲基亚硝胺检出率最高,为90%;N-亚硝胺吡咯烷、N-二乙基亚硝胺和N-二丁基亚硝胺检出率分别为15%、10%和10%。结论 采用水蒸气蒸馏联合DLLME优化即食水产制品中N-亚硝胺类化合物的前处理方法,可满足检测要求。
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陈婧
王立媛
胡争艳
汤鋆
吴平谷
关键词 N-亚硝胺类化合物即食水产制品水蒸汽蒸馏提取液液微萃取气相色谱-三重四极杆质谱    
AbstractObjective To optimize the pretreatment method of N-nitrosamine compounds in ready-to-eat aquatic products. Methods Market-sold ready-to-eat aquatic products were collected, homogenized and distilled by steam. The samples were extracted for 10 minutes using dispersive liquid-liquid microextraction (DLLME) with ethanol, trichloromethane and sodium chloride (3.0 g). After centrifugation, the organic phase in the lower layer was collected and subjected to gas chromatography-tandem mass spectrometry (GC-MS/MS). The six common N-nitrosamine compounds were determined in ready-to-eat aquatic products using multiple reaction monitoring mode (MRM) and quantified by the internal standard method. Results The optimized method exhibited a good linear relationship at concentrations of 10.0 to 500 μg/L for determination of 6 N-nitrosamine compounds (correlation coefficient of greater than 0.999), with 0.05 to 0.60 μg/kg limit of detection, 0.15 to 1.60 μg/kg limit of quantitation, mean spiked recovery rates of 71.8% to 108.9%, and relative standard deviations of 1.4% to 8.6%. N-Nitrosodimethylamine showed the highest detection rate in 20 market-sold ready-to-eat aquatic products (90%), and the detection rates of N-Nitrosopyrrolidine, N-Nitrosodiethylamine and N-dibutylnitrosamine were 15%, 10% and 10%, respectively. Conclusion Steam distillation combined with DLLME may optimize the pretreatment method of N-nitrosamine compounds in ready-to-eat aquatic products and meet the measurement requirements.
Key wordsN-nitrosamine compound    ready-to-eat aquatic product    steam distillation extraction    liquid-liquid microextraction    gas chromatography-tandem mass spectrometry
收稿日期: 2023-06-05      修回日期: 2023-07-20      出版日期: 2023-08-10
中图分类号:  R155.5  
基金资助:2019年广东省重点领域研发计划项目(2019B020212001)
通信作者: 吴平谷,E-mail:pgwu@cdc.zj.cn   
作者简介: 陈婧,硕士,技师,主要从事食品理化检测技术研究工作
引用本文:   
陈婧, 王立媛, 胡争艳, 汤鋆, 吴平谷. 即食水产制品N-亚硝胺类化合物检测的样品处理方法优化研究[J]. 预防医学, 2023, 35(8): 726-731.
CHEN Jing, WANG Liyuan, HU Zhengyan, TANG Jun, WU Pinggu. Optimization of pretreatment methods for N-nitrosamine compounds in ready-to-eat aquatic products. Preventive Medicine, 2023, 35(8): 726-731.
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http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2023.08.018      或      http://www.zjyfyxzz.com/CN/Y2023/V35/I8/726
[1] MEY E D,MAERE H D,PAELINCK H,et al.Volatile N-nitrosamines in meat products:potential precursors,influence of processing,and mitigation strategies[J].Crit Rev Food Sci Nutr,2015,57(13):2909-2923.
[2] 中华人民共和国国家卫生健康委员会,国家市场监督管理总局.食品安全国家标准食品中污染物限量:GB 2762—2022[S].北京:中国标准出版社,2022.
[3] QIU Y,CHEN J H,YU W,et al.Contamination of Chinese salted fish with volatile N-nitrosamines as determined by QuEChERS and gas chromatography-tandem mass spectrometry[J].Food Chem,2017,232:763-769.
[4] 夏日耀,梁棋,杜莲朵,等.GC-FID法同时测定腌制鱼干中9种N-亚硝胺类化合物[J].食品工业科技,2020,41(10):213-223.
[5] 翟孟婷,王宗义,徐芮,等.碱液处理-活性炭柱固相萃取结合GC-MS/MS法检测鱼干、虾皮和虾仁中8种N-亚硝胺[J].质谱学报,2018,39(3):351-359.
[6] 中华人民共和国国家卫生和计划生育委员会,国家食品药品监督管理总局.食品安全国家标准食品中N-亚硝胺类化合物的测定:GB 5009.26—2016[S].北京:中国标准出版社,2016.
[7] ALMEIDA C,FERNANDES J O,CUNHA S C.A novel dispersive liquid-liquid microextraction (DLLME) gas chromatography-mass spectrometry (GC-MS) method for the determination of eighteen biogenic amines in beer[J].Food Control,2012,25(1):380-388.
[8] LI F,LUO J W,ZHU B Q,et al.Pretreatment methods for the determination of antibiotics residues in food samples and detected by liquid chromatography coupled with mass spectrometry detectors:a review[J].J Chromatogr Sci,2022,60(10):991-1003.
[9] MUHAMMAD S.Dispersive liquid-liquid microextraction:evolution in design,application areas,and green aspects[J/OL].Trac-Trend Anal Chem,2022,152[2023-07-20].https://doi.org/10.1016/j.trac.2022.116636.
[10] 刘方征,任雨鑫,张丽萍,等.饱和盐辅助-分散液液微萃取-气相色谱-串联质谱法快速筛查啤酒中氨基甲酸乙酯与9种挥发性亚硝胺[J].食品安全质量检测学报,2022,13(12):3945-3952.
[11] 孔祥一,林鹏,方恩华,等.食品中亚硝胺类化合物分析技术研究进展[J].分析科学学报,2020,36(4):597-605.
[12] RAMEZANI H,HOSSEINI H,KAMANKESH M,et al.Rapid determination of nitrosamines in sausage and salami using microwave-assisted extraction and dispersive liquid-liquid microextraction followed by gas chromatography-mass spectrometry[J].Eur Food Res Technol,2015,240(2):441-450.
[13] JUNG-EUN S,JONG-EUN P,LEE Y,et al.Effect of cooking method on the concentrations of volatile N-nitrosamines in various food products[J/OL].J Food Process Pres,2022,46(7)[2023-07-20].https://doi.org/10.1111/jfpp.16590.
[14] 王艳丽,梁秀清,陈倩倩,等.通过式固相萃取-气相色谱-串联质谱法测定动物源性食品中11种N-亚硝胺类化合物[J].肉类研究,2023,37(3):33-39.
[15] 陈丽香,陈嘉敏,陈燕敏,等.QuEChERS-气相色谱-三重四极杆串联质谱法测定水产干制品中9种N-亚硝胺类化合物[J].现代食品科技,2021,37(8):295-301,257.
[16] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.合格评定化学分析方法确认和验证指南:GB/T 27417—2017[S].北京:中国标准出版社,2017.
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