摘要
建立水蒸气蒸馏-气相色谱-质谱联用法同时测定干制水产品中3种N-亚硝胺(NAs)痕量检测方法.通过系统对比并优化干制水产品中NAs的前处理方法,最终确立水蒸气蒸馏法提取结合GC-MS/MS检测技术. NAs在5~400 ng·mL^(-1)范围内呈现良好线性关系(R^(2)>0.999),方法检出限和定量限分别为0.3和1.0μg·kg^(-1).加标回收实验表明,在1~15μg·kg^(-1)添加水平内,平均回收率为67.4%~120%,相对标准偏差为0.82%~7.19%,表明方法具有良好的准确度和精密度.实际样品检测发现N-亚硝基二甲胺检出率和超标率最高,污染情况最为严重,在各类型的干制水产品中均有不同程度的检出.风险评估结果表明,NAs平均癌症风险范围为1.32×10^(-7)~1.16×10^(-5),其中N-亚硝基二甲胺和N-亚硝基二乙胺存在潜在的癌症风险,应对其进行风险管控.
A method was developed for the simultaneous determination of three N-nitrosamines(NAs)in dried aquatic products by water vapor distillation(WVD)coupled with gas chromatography-mass spectrometry(GC-MS/MS).The pretreatment methods of NAs in dried aquatic products were systematically compared and optimized,and the extraction method by water vapor distillation combined with GC-MS/MS was finally established.The linear range of NAs was 5 to 400 ng·mL^(-1)(R^(2)>0.999),and the limits of detection(LOD)and the limits of quantification(LOQ)of NAs were 0.3 and 1.0μg·kg^(-1),r espectively.The recoveries of NAs in standardized spiked products were as follows.The average recoveries ranged from 67.4%to 120%with the relative standard deviations(RSDs)of 0.82%to 7.19%at the spiked levels of 1 to 15μg·kg^(-1),indicating that the method has good accuracy and precision.The actual sample testing revealed that N-nitrosodimethylamine had the highest detection and exceedance rates and the most serious contamination,and was detected in all types of dried aquatic products in different degrees.The results of risk assessment showed that N-nitrosodimethylamine and N-nitrosodiethylamine have potential cancer risk and should be subject to risk control.
作者
苏家颍
林河通
林振宇
罗芳
刘智禹
汤水粉
陈财珍
陈宇锋
姜琳琳
钱卓真
SU Jiaying;LIN Hetong;LIN Zhenyu;LUO Fang;LIU Zhiyu;TANG Shuifen;CHEN Caizhen;CHEN Yufeng;JIANG Linlin;QIAN Zhuozhen(College of Food Science,Fujian Agriculture and Forestry University,Fuzhou,Fujian 350002,China;Ministry of Education Key Laboratory for Analytical Science of Food Safety and Biology,College of Chemistry,Fuzhou University,Fuzhou,Fujian 350108,China;Key Laboratory of Cultivation and High-Value Utilization of Marine Organisms in Fujian Province,Fisheries Research Institute of Fujian,Xiamen,Fujian 361013,China)
出处
《福州大学学报(自然科学版)》
北大核心
2025年第3期375-382,共8页
Journal of Fuzhou University(Natural Science Edition)
基金
福建省自然科学基金资助项目(2023J011322)
福建省促进海洋与渔业产业高质量发展专项资金项目(FJHYF-L-2023-27)。
关键词
N-亚硝胺
干制水产品
风险评估
气相色谱-质谱联用法
N-nitrosamines
dried aquatic products
risk assessment
gas chromatography-mass spectrometry
