食品科学 ›› 2021, Vol. 42 ›› Issue (16): 281-285.doi: 10.7506/spkx1002-6630-20200716-223

• 安全检测 • 上一篇    下一篇

UPLC-MS/MS法测定黄酒中8 种生物胺

王可利,叶泰,徐斐,曹慧,袁敏,于劲松,阴凤琴,吴秀秀   

  1. (上海食品快速检测工程技术研究中心,上海理工大学医疗器械与食品学院,上海 200093)
  • 发布日期:2021-08-27
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFC1604202); 上海市食品安全风险监测与评估项目(SHXM-00-20180328-4089)

Determination of Eight Biogenic Amines in Huangjiu (Rice Wine) by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Keli, YE Tai, XU Fei, CAO Hui, YUAN Min, YU Jinsong, YIN Fengqin, WU Xiuxiu   

  1. (Shanghai Engineering Research Center for Food Rapid Detection, School of Medical Instrument and Food Engineering, University of Shanghai for Science and Technology, Shanghai 200093, China)
  • Published:2021-08-27

摘要: 建立黄酒中组胺、酪胺、腐胺、色胺、β-苯乙胺、尸胺、精胺、亚精胺共8?种生物胺的超高效液相色谱-串联质谱检测方法。样品衍生化处理后,经C18色谱柱(100.0?mm×2.1?mm,1.7?μm)分离,0.1%甲酸溶液、0.1%甲酸-乙腈溶液作为流动相梯度洗脱,用多反应监测模式下的电喷雾正离子扫描获得质谱数据,并采用内标法进行定量。结果表明:8?种生物胺可在19?min内分离,且在各自质量浓度范围内线性良好,r2均大于0.995?1;检出限为0.25~0.50?ng/mL,定量限为1~2?ng/mL,日内精密度为0.61%~5.68%,日间精密度为0.82%~5.00%;黄酒样品中生物胺的加标回收率在83.56%~117.45%之间,相对标准偏差均低于6.69%。

关键词: 黄酒;生物胺;衍生;超高效液相色谱-串联质谱法

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry method for the determination of eight biogenic amines in Huangjiu (rice wine), including histamine, tyramine, putrescine, tryptamine, β-phenylethylamine, cadaverine, spermine and spermidine, was established. Complete separation of the derivatives of eight biogenic amines was achieved on a C18 chromatographic column (100.0 mm × 2.1 mm, 1.7 μm) by gradient elution with acetonitrile-0.1% formic acid in water as the mobile phase. Mass spectral data were obtained in the multi-reaction monitoring mode by electrospray positive ion scanning. The internal standard method was employed for quantification. The results showed that the eight biogenic amines were separated completely within 19 min?and good linearity was obtained for histamine in the range of 2–1 000 ng/mL and for other amines in the range of 1–1 000 ng/mL (r2 > 0.995 1). The limit of detection (LOD) and the limit of quantification (LOQ) of the method were in the range of 0.25–0.5 and 1–2 ng/mL, respectively. The intraday and interday precision of the proposed method was in the range of 0.61%–5.68% and 0.82%–5.00%, respectively. Satisfactory recoveries for spiked rice wine samples were obtained in the range of 83.56%–117.45% with relative standard deviation (RSD) lower than 6.69%.

Key words: rice wine; biogenic amines; derivatization; ultra-high performance liquid chromatography-tandem mass spectrometry

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