高效液相色谱-质谱/质谱法测定水产品和肉类中9种生物胺
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1江苏省疾病预防控制中心,江苏 南京 210009;2上海迪柯马科技发展有限公司天津分公司, 天津 300401

作者简介:

王溪 女 主管技师 研究方向为食品、化妆品、消毒产品理化检验 E-mail: wangxi_sanjia@163.com

通讯作者:

吉文亮 男 主任技师 研究方向为食品、化妆品、消毒产品理化检验 E-mail: 502869110@qq.com

中图分类号:

R155

基金项目:

江苏省卫生健康委科研课题(Ym2023041)


Determination of 9 biogenic amines in aquatic products and meat by high performance liquid chromatography tandem mass spectrometry
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1Jiangsu Provincial Center for Disease Control and Prevention, Jiangsu Nanjing 210009, China;2Shanghai Dikma Technology Development Co., Ltd. Tianjin Branch, Tianjin 300401, China

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    摘要:

    目的 建立快速测定水产品(鱼、虾、贝)和肉类(猪肉、牛肉、羊肉)中9种生物胺含量的高效液相色谱-质谱/质谱法。方法 样品先加入乙腈沉淀蛋白,再用0.5%三氯乙酸溶液提取,正己烷除脂后取下层样品溶液稀释后用DVB(100 mg/3 mL)固相萃取小柱净化,以70%乙腈+30%水(含100 mmol/L甲酸铵和0.5%甲酸)和90%乙腈+10%水作为流动相梯度洗脱,目标物经ACQUITY UPLC? BEH Amide柱(1.7 μm,2.1 mm ×100 mm)分离,使用电喷雾离子源、正离子多反应监测模式进行检测,内标法定量。结果 腐胺、尸胺、精胺、亚精胺在5~500 ng/mL,组胺、酪胺、色胺、章胺、β-苯乙胺在0.5~50 ng/mL范围内线性关系良好,相关系数r均>0.996。腐胺、尸胺、精胺、亚精胺检出限为1 mg/kg,定量限为3 mg/kg,组胺、酪胺、色胺、章胺、β-苯乙胺的检出限为0.1 mg/kg,定量限为0.3 mg/kg。水产品和肉类低、中、高3个添加浓度水平的加标回收率为70.6%~119%,相对标准偏差均<10%(n=6)。结论 该方法操作简便,准确可靠、灵敏度高,适用于水产品(鱼、虾、贝)和肉类(猪肉、牛肉、羊肉)中生物胺的检测。

    Abstract:

    Objective To establish a high-performance liquid chromatography tandem mass spectrometry method for rapid determination of nine biogenic amines in aquatic products (fish, shrimp, shellfish) and meat (pork, beef, mutton) based on non derivatized passing through nsolid-phase extraction pretreatment technology.Methods Acetonitrile was used to precipitate the protein in the sample, then 0.5% trichloroacetic acid solution was used for extraction. After removing the lipid with n-hexane, lower layer of the sample solution was diluted and purified by passing through a DVB (100 mg/3 mL) solid-phase extraction column. 70% acetonitrile+30% water (containing 100 mmol/L ammonium formate and 0.5% formic acid) and 90% acetonitrile+10% water were used as mobile phase for gradient elution. The target substance was eluted by ACQUITY UPLC? BEH Amide column (1.7 μm, 2.1 mm×100 mm) was used for separation. Electrospray ion source and positive ion multi reaction monitoring mode were used for detection, and internal standard method was used for quantification.Results The linear relationship between putrescine, cadaverine, spermine, and spermine was good within the range of 5-500 ng/mL, while histamine, tyramine, serotonin, phenylethylamine, and β-phenylethylamine were good within the range of 0.5-50 ng/mL, with correlation coefficients r>0.996. The detection limit of putrescine, cadaverine, spermine, and spermidine was 1 mg/kg, and the quantification limit was 3 mg/kg. The detection limit of histamine, tyramine, serotonin, phenylethylamine, and β-phenylethylamine was 0.1 mg/kg, and the quantification limit was 0.3 mg/kg. The spiked recovery rates of low, medium, and high concentrations in aquatic and meat products ranged from 70.6% to 119%, with relative standard deviations less than 10% (n=6).Conclusion This method was easy to operate, accurate, reliable, and highly sensitive, and was suitable for the detection of biogenic amines in aquatic products (fish, shrimp, shellfish) and meat (pork, beef, mutton).

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王溪,李文斌,马利静,吉文亮.高效液相色谱-质谱/质谱法测定水产品和肉类中9种生物胺[J].中国食品卫生杂志,2025,37(9):817-827.

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  • 收稿日期:2025-06-25
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  • 在线发布日期: 2026-03-02
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