固相萃取-高效液相色谱-串联质谱法测定植物源食品中嗪氨灵的残留量
Determination of triforine residues in plant-derived food by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry
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摘要: 建立了固相萃取-液相色谱-串联质谱测定植物源食品（大米、大豆、菠菜、番茄、辣椒、蘑菇等）中嗪氨灵残留量的检测方法。试样用乙腈均质提取,采用石墨化碳黑/氨基柱（ENVI-Carb/NH2）净化后,用多反应监测（MRM）正离子扫描方式进行检测,外标法定量。结果表明,嗪氨灵在21000 ng/m L范围内呈线性关系良好,方法的检出限（S/N=3）为0.51.5μg/kg,定量限（S/N=10）为1.64.9μg/kg,加标平均回收率范围为68.4%109.0%,相对标准偏差（RSD）为4.38%13.5%。方法的选择性好,抗干扰能力强,能满足国内外法规的要求,可以为植物源食品中嗪氨灵残留的检测提供技术支持。Abstract: A method was developed for the simultaneous determination of triforine residue in various plant- derived foods( such as rice,soybean,spinach,tomato,pepper,and mushroom) by solid phase extraction- liquid chromatography- tandem mass spectrometry.The samples were extracted by acetonitrile,cleaned- up with an ENVI- Carb / NH2solid- phase extractor,and determined by high performance liquid chromatography- tandem mass spectrometry( HPLC- MS / MS) using external standard method with positive polarity mode under multi- reaction monitoring( MRM) scan type.The method showed good linearity in the range from 2 to 1000 ng / m L.The limits of detection( LODs,S / N = 3) varies over the range of 0.5 to 1.5 μg / kg,and limits of quantification( LOQs,S / N = 10) ranged from 1.6 to 4.9 μg / kg.The average recoveries in different matrices were in the range of68.4% ~109.0%,with relative standard deviations( RSDs) of 4.38% ~13.5%.This method was selective without interference and reliable for meeting the requirements of the domestic and international legislation. The method was suitable for triforine determination in plant- derived food.
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