陈其煌. 基于PRiME HLB净化高效液相色谱-串联质谱法测定饲料中苯乙醇胺A[J]. 福建农业科技, 2021, 51(2): 24-31. DOI: 10.13651/j.cnki.fjnykj.2021.02.005
    引用本文: 陈其煌. 基于PRiME HLB净化高效液相色谱-串联质谱法测定饲料中苯乙醇胺A[J]. 福建农业科技, 2021, 51(2): 24-31. DOI: 10.13651/j.cnki.fjnykj.2021.02.005
    CHEN Qi-huang. Determination of Phenylethanolamine A in Feed Based on High Performance Liquid Chromatography-Tandem Mass Spectrometry After Purified by PRiME HLB[J]. Fujian Agricultural Science and Technology, 2021, 51(2): 24-31. DOI: 10.13651/j.cnki.fjnykj.2021.02.005
    Citation: CHEN Qi-huang. Determination of Phenylethanolamine A in Feed Based on High Performance Liquid Chromatography-Tandem Mass Spectrometry After Purified by PRiME HLB[J]. Fujian Agricultural Science and Technology, 2021, 51(2): 24-31. DOI: 10.13651/j.cnki.fjnykj.2021.02.005

    基于PRiME HLB净化高效液相色谱-串联质谱法测定饲料中苯乙醇胺A

    Determination of Phenylethanolamine A in Feed Based on High Performance Liquid Chromatography-Tandem Mass Spectrometry After Purified by PRiME HLB

    • 摘要: 建立高效液相色谱-串联质谱法测定饲料中苯乙醇胺A的分析方法。样品用80%(V:V)乙腈水溶液提取,经PRiME HLB净化后,采用高效液相色谱-串联质谱法测定,外标法定量。以0.1%甲酸水溶液和甲醇作为流动相,用Hypersil GOLD C18色谱柱(1.9 μm,2.1 mm×100 mm)进行梯度洗脱,采用电喷雾离子源(ESI+)、正离子扫描多反应监测(MRM)模式进行定性和定量分析。结果表明:苯乙醇胺A在5.0~200.0 ng·mL-1的范围内线性关系良好(r=0.999 2)。在10.0、20.0、50.0 μg·kg-1添加水平下的回收率为82.2%~91.5%,相对标准偏差(n=6)为6.8%~8.5%,检出限(以信噪比>3计)为0.1 μg·kg-1,定量限(以信噪比>10计)为0.3 μg·kg-1。该方法精密度好,灵敏度高,可用于大批量快速准确测定饲料中的苯乙醇胺A,有效提高工作效率。

       

      Abstract: A analytical method for the determination of phenylethanolamine A in feed by high performance liquid chromatography-tandem mass spectrometry was established. The samples were extracted with 80% (V:V) acetonitrile aqueous solution. After purified by PRiME HLB, the samples were determined by high performance liquid chromatography-tandem mass spectrometry and quantified by external standard method. Then, the gradient elution was performed through Hypersil GOLD C18 chromatographic column (1.9 μm, 2.1 mm×100 mm) by using 0.1% formic acid aqueous solution and methanol as the mobile phase. And the qualitative and quantitative analysis was carried out by using the modes of electrospray ionization (ESI+) and positive-ion scanning multiple reaction monitoring (MRM). The results showed that phenylethanolamine A had a good linear relationship in the range of 5.0~200.0 ng·mL-1 (r=0.999 2). The recoveries were 82.2% to 91.5% at the supplemented levels of 10.0, 20.0 and 50.0 μg·kg-1, the relative standard deviations (n=6) were 6.8% to 8.5%, the limits of detection (the SNR being greater than 3) were 0.1 μg·kg-1, and the limits of quantification (the SNR being greater than 10) were 0.3 μg·kg-1. The method had good precision and high sensitivity, and could be used for the rapid and accurate determination of phenylethanolamine A in large quantities, which would effectively improve the work efficiency.

       

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