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投稿时间:2026-01-06
投稿时间:2026-01-06
中文摘要: 该研究建立可同步测定二甲胺、三甲胺、氧化三甲胺的非抑制型离子色谱法。试样经质量浓度为1%的三氯乙酸溶液提取,三氯甲烷净化,结合超声辅助提取和高速冷冻离心去除蛋白干扰,采用Dionex Ionpac CS 17阳离子交换色谱柱进行分离,以3.08 mmol/L甲烷磺酸为流动相,在0.8 mL/min流速下于15 min内实现3种目标胺的完全分离。该方法的二甲胺、三甲胺和氧化三甲胺的定量限分别为0.17、0.21、0.25 mg/g。进一步结合液相色谱-质谱法,构建了适用于水产品及干制品中N-二甲基亚硝胺及其前体物的多目标物检测分析体系。基于上述检测分析体系,系统监测鳕鱼片生产加工过程中氧化三甲胺、二甲胺、三甲胺和N-二甲基亚硝胺的含量,探究前体物质与N-二甲基亚硝胺间二者的变化规律,以期为阐明干制水产品加工过程中N-二甲基亚硝胺的形成机制及关键控制点提供方法学依据与理论支撑。
中文关键词: 离子色谱法 鳕鱼片 N-二甲基亚硝胺 生物胺 液相色谱-串联质谱法
Abstract:This study established a non-suppressed ion chromatography method capable of simultaneously measuring dimethylamine,trimethylamine,and trimethylamine N-oxide. The sample was extracted with a 1%trichloroacetic acid solution,purified with chloroform,and subjected to ultrasonic-assisted extraction and high-speed refrigerated centrifugation to remove protein interference. Separation was performed on a Dionex Ionpac CS 17 cation exchange column using 3.08 mmol/L methanesulfonic acid as the mobile phase at a flow rate of 0.8 mL/min,achieving complete separation of the three target amines within 15 min. The limits of quantification for dimethylamine,trimethylamine,and trimethylamine N-oxide were 0.17,0.21,and0.25 mg/g,respectively. Furthermore,combined with liquid chromatography-mass spectrometry,a multi-target detection and analysis system suitable for N-nitrosodimethylamine and its precursors in aquatic products and dried products was established. Based on this detection system,the contents of trimethylamine N-oxide,dimethylamine,trimethylamine,and N-nitrosodimethylamine in cod fillets during processing were systematically monitored,and the variation patterns between the precursors and N-nitrosodimethylamine were explored. This provides a methodological basis and theoretical support for elucidating the formation mechanism and key control points of N-nitrosodimethylamine during the processing of dried aquatic products.
keywords: ion chromatography (IC) cod fillet N-nitrosodimethylamine biogenic amines liquid chromatography-tandem mass spectrometry (LC-MS/MS)
文章编号:202617022 中图分类号: 文献标志码:
基金项目:福建省自然科学基金(2023J011322);厦门市自然科学基金(3502Z202374095);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)
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