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中国精品科技期刊2020
蒋林蓉, 徐志伟, 曾敏, 黄杰英, 徐莉, 符传军, 庞道标, 李实飞. 改进的QuEChERS结合RPLC-TMS测定水产品中生物胺的研究[J]. 食品工业科技, 2016, (22): 68-72. DOI: 10.13386/j.issn1002-0306.2016.22.005
引用本文: 蒋林蓉, 徐志伟, 曾敏, 黄杰英, 徐莉, 符传军, 庞道标, 李实飞. 改进的QuEChERS结合RPLC-TMS测定水产品中生物胺的研究[J]. 食品工业科技, 2016, (22): 68-72. DOI: 10.13386/j.issn1002-0306.2016.22.005
JIANG Lin-rong, XU Zhi-wei, ZENG Min, HUANG Jie-ying, XU Li, FU Chuan-jun, PANG Dao-biao, LI Shi-fei. Determination of biogenic amines in aquatic products by modified Qu ECh ERS method and liquid chromatography-mass spectrometry[J]. Science and Technology of Food Industry, 2016, (22): 68-72. DOI: 10.13386/j.issn1002-0306.2016.22.005
Citation: JIANG Lin-rong, XU Zhi-wei, ZENG Min, HUANG Jie-ying, XU Li, FU Chuan-jun, PANG Dao-biao, LI Shi-fei. Determination of biogenic amines in aquatic products by modified Qu ECh ERS method and liquid chromatography-mass spectrometry[J]. Science and Technology of Food Industry, 2016, (22): 68-72. DOI: 10.13386/j.issn1002-0306.2016.22.005

改进的QuEChERS结合RPLC-TMS测定水产品中生物胺的研究

Determination of biogenic amines in aquatic products by modified Qu ECh ERS method and liquid chromatography-mass spectrometry

  • 摘要: 采用改进的Qu ECh ERS方法,利用液相色谱-串联质谱(RPLC-TMS)检测,建立了几种水产品中生物胺的分析方法。样品用乙腈+甲醇(9+1)提取,无水硫酸钠除去水分,经乙二胺-N-丙基硅烷(PSA)和C18混合粉末净化,采用HILIC柱,以乙腈/1%甲酸水溶液为流动相梯度洗脱进行液相色谱分离。质谱分析采用电喷雾正离子电离,多反应监测模式,外标法定量。结果显示6种生物胺在10200 ng/m L范围线性关系良好。方法的定量限(LOQ,信噪比为10)为0.10 mg/kg。加标水平在0.10 mg/kg时,鱼、虾、蟹及鱿鱼四种阴性基质中加标的回收率在74.18%90.15%之间,相对标准偏差(RSD,n=6)在2.22%8.04%之间。结果表明本方法简便、快速、安全、适用于水产品中生物胺含量的定性和定量检测。 

     

    Abstract: A modified Qu ECh ERS method followed by liquid chromatography- tandem mass spectrometric analysis was developed for the determination of biogenic amines in aquatic products. The samples was diluted with acetonitrile / methanol solution( 9 /1) and cleaned up with primary secondary amine( PSA) and Octadecylsilane( C18) sorbent.The separation of biogenic amines was performed by hydrophilic interaction liquid chromatography( HILIC) column and gradiently eluting with acetonitrile/formic acid- water( 1%) without derivatization. Biogenic amines were analyzed by positive electrosprary ionization( ESI~+) tandem mass spectrometry under multiple reaction monitoring( MRM) mode.Quantification was achieved using external standard method.The linearities were excellent in the range of 10~200 ng / m L.The limits of quantification( LOQ,S / N = 10) were 0.10 mg / kg.The recoveries of biogenic amines spiked in matrices were between 74.18% and 90.15% at the spiked levels of 0.10 mg / kg. The relative standard deviations( RSDs,n = 6) were in the range of 2.22% ~8.04%.The method( quick,easy,safe) could meet the requirements of the daily work for the determination of biogenic amines in aquatic products.

     

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