挥发性离子对反相液相色谱-串联质谱法检测冷链鱼虾中16 种生物胺

doi:10.7506/spkx1002-6630-20241101-010

食品科学 ›› 2025, Vol. 46 ›› Issue (10): 282-289.doi: 10.7506/spkx1002-6630-20241101-010

挥发性离子对反相液相色谱-串联质谱法检测冷链鱼虾中16 种生物胺

吴建欣，王宗义，于淼，毕桂宾，张巍青，董子琦，马小童

（1.北京农学院食品科学与工程学院，农产品有害微生物及农残安全检测与控制北京市重点实验室，北京 102206；2.广州禾信仪器股份有限公司，广东广州 510535）

出版日期:2025-05-25 发布日期:2025-05-07
基金资助:
北京市教委都市农林学交叉学科平台建设项目（2023）

Determination of 16 Biogenic Amines in Cold-Chain Fish and Shrimp by Volatile Ion-Pair Reversed-Phase Liquid Chromatography-Tandem Mass Spectrometry

WU Jianxin, WANG Zongyi, YU Miao, BI Guibin, ZHANG Weiqing, DONG Ziqi, MA Xiaotong

(1. 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 102206, China; 2. Guangzhou Hexin Instrument Co. Ltd., Guangzhou 510535, China)

Online:2025-05-25 Published:2025-05-07

摘要/Abstract

摘要： 针对冷链鱼虾产品，基于液相色谱-串联质谱法建立无衍生化检测二甲胺、三甲胺、氧化三甲胺、章鱼胺、多巴胺、酪胺、5-羟色胺、苄胺、腐胺、尸胺、组胺、胍丁胺、2-苯乙胺、色胺、亚精胺和精胺共16 种生物胺的新方法。样品经1%（V/V）甲酸-80%（V/V）乙腈溶液均质提取，正己烷除脂，使用Waters XSelectTM HSS T3柱，以5 mmol/L九氟戊酸溶液和5 mmol/L九氟戊酸-乙腈溶液为流动相进行梯度洗脱，进行挥发性离子对反相色谱分离，在电喷雾电离离子源正离子模式下，以多反应监测模式进行质谱检测，以二甲胺-D6和1,7-二氨基庚烷为内标进行定量。结果表明，各生物胺均能有效分离，在10～1 000 ng/mL范围内线性良好，R2＞0.995，检出限为0.15～1.50 mg/kg，定量限为0.5～5.0 mg/kg，平均加标回收率为81.15%～109.90%，相对标准偏差均小于10%。实际样品检测结果表明，市售冷链鱼虾产品中除色胺、5-羟色胺、多巴胺和章鱼胺外，其他12 种生物胺均有不同程度检出。该方法样品前处理简单、灵敏度高、准确性和精密度良好，可为无衍生的液相色谱-串联质谱法高效检测生物胺与以生物胺为标志物的冷链鱼虾产品质量综合评价提供技术参考。

关键词: 生物胺；冷链鱼虾；挥发性离子对；液相色谱-串联质谱法

Abstract: A new method for the determination of 16 biogenic amines (BAs) including dimethylamine, trimethylamine, trimethylamine oxide, octopamine (OA), dopamine (DA), tyramine (TYR), 5-hydroxytryptamine (5-HT), benzylamine, putrescine, cadaverine, histamine, agmatine, 2-phenylethylamine, tryptamine, spermidine and spermine in cold-chain fish and shrimp products was established using liquid chromatography-tandem mass spectrometry (LC-MS/MS) without derivatization. Samples were extracted by homogenizing with a solvent mixture of 1% (V/V) formic acid-80% (V/V) acetonitrile solution and degreased with n-hexane. Then, volatile ion-pairing reversed-phase chromatographic separation was carried out on a Waters XSelectTM HSS T3 column with gradient elution using a mobile phase consisting of 5 mmol/L nonafluoropentanoic acid (NFPA) solution (A) and 5 mmol/L NFPA in acetonitrile (B), and mass spectrometric detection was performed using an electrospray ionization source in the positive ion mode with multiple reaction monitoring (MRM). Dimethylamine-d6 and 1,7-diaminoheptane were used as internal standards for quantification. The results showed that all 16 BAs were well separated chromatographically and each BA exhibited good linearity in the concentration range of 10 to 1 000 ng/mL, with correlation coefficients (R2) greater than 0.995. The limits of detection (LODs) ranged from 0.15 to 1.50 mg/kg and the limits of quantification (LOQs) were in the range of 0.5–5.0 mg/kg. The average recoveries for spiked samples were between 81.15% and 109.90%, with relative standards deviations (RSDs) of less than 10%. All analytes except TRY, 5-HT, DA and OA were detected in commercial cold-chain fish and shrimp products. This method, characterized by simple sample preparation, high sensitivity, good accuracy and precision, provides valuable technical references for the highly efficient detection of BAs via underivatized LC-MS/MS, as well as for comprehensive quality evaluation of cold-chain fish and shrimp products based on BAs as markers.

Key words: biogenic amines; cold-chain fish and shrimp; volatile ion-pair; liquid chromatography-tandem mass spectrometry

中图分类号:

O657.63

吴建欣，王宗义，于淼，毕桂宾，张巍青，董子琦，马小童. 挥发性离子对反相液相色谱-串联质谱法检测冷链鱼虾中16 种生物胺[J]. 食品科学, 2025, 46(10): 282-289.

WU Jianxin, WANG Zongyi, YU Miao, BI Guibin, ZHANG Weiqing, DONG Ziqi, MA Xiaotong. Determination of 16 Biogenic Amines in Cold-Chain Fish and Shrimp by Volatile Ion-Pair Reversed-Phase Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2025, 46(10): 282-289.

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挥发性离子对反相液相色谱-串联质谱法检测冷链鱼虾中16 种生物胺

Determination of 16 Biogenic Amines in Cold-Chain Fish and Shrimp by Volatile Ion-Pair Reversed-Phase Liquid Chromatography-Tandem Mass Spectrometry

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