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| 液相色谱-串联质谱法检测干熏鱼中的4种非挥发性亚硝胺 |
| Determination of four non-volatile nitrosamines in dried smoked fish by liquid chromatography-tandem mass spectrometry |
| 投稿时间：2025-01-16 修订日期：2025-03-10 |
| DOI： |
| 中文关键词: 非挥发性N-亚硝胺 干熏鱼 液相色谱-串联质谱法 |
| 英文关键词:non-volatile N-nitrosamine dried smoked fish liquid chromatography-tandem mass spectrometry |
| 基金项目:北京市都市农林学交叉学科平台建设项目(2023); 北京农学院教改重点项目-服务乡村振兴专业能力实训课程体系的构建与教学实践(5046516654/149) |
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| Author | Institution |
| CHEN Chen | Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture |
| WU Jian-Xin | Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture |
| WANG Zong-Yi | Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture;Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture |
| ZHANG Wei-Qing | Guangzhou Hexin Instrument Co,Ltd |
| YANG Li-Hua | Guangzhou Hexin Instrument Co,Ltd |
| MA Xiao-Tong | Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture |
| DONG Zi-Qi | Beijing Laboratory of Food Quality and Safety,Beijing Key Laboratory of Agricultural Product Detection and Control for Spoilage Organisms and Pesticides,College of Food Sciences and Engineering,Beijing University of Agriculture |
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| 中文摘要: |
| 目的 建立液相色谱-串联质谱测定干薰鱼中N-亚硝基脯氨酸（Nitrosoproline，NPRO）、N-亚硝基肌氨酸（Nitrososarcosine，NSAR）、N-亚硝基-噻唑烷-4-羧酸（Nitroso-Thiazolidine-4-Carboxylic Acid，NTCA）和N-亚硝基-2-甲基-噻唑烷-4-羧酸（Nitroso-2-Methyl-Thiazolidine 4-Carboxylic Acid，NMTCA）4种非挥发性N-亚硝胺（Non volatile nitrsoamine, NVNA）的新方法。方法 样品经乙腈提取，正己烷脱脂，MORHCHEM Caprisil C18-AQ（5 μm, 4.6?250 mm）色谱柱分离，采用多反应监测模式进行液相色谱-串联质谱检测，基质标曲，外标法定量。结果 4种NVNA在1, 4, 10, 50 ng/mL分别至800 ng/mL的范围内线性良好，R2>0.996，检出限为1.36~56.17 μg/kg，定量限为4.52~187.2 μg/kg，加标回收率为90.34%~103.6%，相对标准偏差为1.75%~6.47%。实际应用显示，市售干薰鱼样品中均有不同程度、不同种类的NVNA检出，其中具有弱致癌性的NSAR检出率和含量都较高。结论 本方法样品前处理简单、准确性好、精密度高，能够满足干薰鱼中4种NVNA的同步测定，为干薰鱼制品中NVNA的污染监测与控制提供了有价值的技术参考。 |
| 英文摘要: |
| ABSTRACT:Objective To establish a new method for the determination of four non-volatile N-nitrosamines (NVNA), Nitrosoproline (NPRO), Nitrososarcosine (NSAR), Nitroso-Thiazolidine-4-Carboxylic Acid (NTCA) and Nitroso-Thiazolidine-4-Carboxylic Acid (NMTCA), in dried smoked fish products by liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by acetonitrile, degreased with n-hexane, separated on a MORHCHEM Caprisil C18-AQ(5 μm, 4.6?250 mm)column, and detected by liquid chromatography-tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring (MRM) mode, and quantified by the external standard method of matrix standard curve. Results The linearity of the four NVNA was good in ranges of 1,4,10 or 50 - 800 ng/mL with R2>0.996, the detection limits were 1.36-56.17 μg/kg, the quantification limits were 4.52-187.2 μg/kg, and the spiked recoveries of 4 NVNA ranged from 90.34%- 103.6% with the relative standard deviations (RSDs) of 1.75%-6.47%. Practical applications showed that NVNAs were detected in commercially available samples of the dried smoked fish at different levels and in different species, with the weakly carcinogenic NSAR being detected at higher rates and levels. Conclusion This method is simple in sample pretreatment, good in accuracy and high in precision, which can meet the simultaneous determination of 4 NVNA in dried smoked fish, and provides a valuable technical reference for the regulation and control of the NVNA contamination level in dried smoked fish products. |
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