Zhongguo youzhi (Nov 2022)

超高效液相色谱-串联质谱法测定植物油中 4种杂环胺含量Determination of four heterocyclic aromatic amines in vegetable oils by ultra-performance liquid chromatography-tandem mass spectrometry

  • 任丹丹1，陈修红2，孙东哲1，王满意1，于雷3，王翔宇1 REN Dandan1, CHEN Xiuhong2, SUN Dongzhe1, WANG Manyi1, YU Lei3, WANG Xiangyu1

DOI
https://doi.org/10.19902/j.cnki.zgyz.1003-7969.210465
Journal volume & issue
Vol. 47, no. 11
pp. 121 – 125

Abstract

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建立超高效液相色谱-串联质谱法（UPLC-MS/MS）测定植物油中4种杂环胺(MeIQx、4，8-DiMeIQx、7,8-DiMeIQx、PhIP)的分析方法。样品经含1%氨水乙腈提取、乙腈饱和的正己烷脱脂后，利用PCX固相萃取柱进行净化。净化后的样品采用乙腈和10 mmol/L甲酸铵溶液作为流动相进行梯度洗脱，在正离子模式下以电喷雾电离串联质谱对杂环胺的定量离子和定性离子进行监测，并利用内标法进行定量。结果表明：4种杂环胺在0.5~100.0 ng/mL范围内线性关系良好，相关系数均大于0.99，方法检出限为0.01~0.04 μg/kg，定量限为0.03~0.13 μg/kg；在1.0、5.0、10.0 μg/kg的加标水平下，杂环胺的平均回收率在64.5%~96.5%之间，相对标准偏差在2.83%~8.52%之间。本方法快速、准确、灵敏，可应用于植物油中4种杂环胺的同时检测。 A method for determination of four heterocyclic aromatic amines(MeIQx, PhIP, 4,8-DiMeIQx and 7,8-DiMeIQx) in vegetables oils by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established. The samples were extracted by acetonitrile containing 1% ammonium hydroxide, defatted by n-hexane saturated by acetonitrile, followed by the purification with PCX solid phase extraction column. Then the heterocyclic aromatic amines in the extracts were separated by a gradient elution of acetonitrile and 10 mmol/L ammonium formate aqueous solution, then quantitative and qualitative ion of heterocyclic aromatic amines were monitored by electrospray ionization tandem mass spectrometry in positive ion mode, and quantified by internal standard method. The results showed that all of the analytes showed good linearity in the range of 05-1000 ng/mL and the correlation coefficients (r2) were all above 0.99. The limits of detection for heterocyclic aromatic amines were 0.01-0.04 μg/kg, and the limits of quantification were 0.03-0.13 μg/kg. The average recoveries of heterocyclic aromatic amines at spiked levels of 1.0, 5.0, 10.0 μg/kg ranged from 64.5% to 96.5%, with the relative standard deviations of 2.83%-8.52%. The method is rapid, accurate and sensitive, and is suitable for the determination of four heterocyclic aromatic amines in vegetable oils.

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