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中国精品科技期刊2020
闵宇航,黄璐瑶,余晓琴,等. 超高效液相色谱-串联质谱法测定酱卤肉制品中1-甲基咪唑、2-甲基咪唑及4-甲基咪唑[J]. 食品工业科技,2021,42(10):261−266. doi: 10.13386/j.issn1002-0306.2020080139.
引用本文: 闵宇航,黄璐瑶,余晓琴,等. 超高效液相色谱-串联质谱法测定酱卤肉制品中1-甲基咪唑、2-甲基咪唑及4-甲基咪唑[J]. 食品工业科技,2021,42(10):261−266. doi: 10.13386/j.issn1002-0306.2020080139.
MIN Yuhang, HUANG Luyao, YU Xiaoqin, et al. Simultaneous Determination of 1-Methylimidazole, 2-Methylimidazole and 4-Methylimidazole in Sauced Meat Products by Ultra High Performance Liquid Chromatograhpy-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(10): 261−266. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306. 2020080139.
Citation: MIN Yuhang, HUANG Luyao, YU Xiaoqin, et al. Simultaneous Determination of 1-Methylimidazole, 2-Methylimidazole and 4-Methylimidazole in Sauced Meat Products by Ultra High Performance Liquid Chromatograhpy-Tandem Mass Spectrometry[J]. Science and Technology of Food Industry, 2021, 42(10): 261−266. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306. 2020080139.

超高效液相色谱-串联质谱法测定酱卤肉制品中1-甲基咪唑、2-甲基咪唑及4-甲基咪唑

Simultaneous Determination of 1-Methylimidazole, 2-Methylimidazole and 4-Methylimidazole in Sauced Meat Products by Ultra High Performance Liquid Chromatograhpy-Tandem Mass Spectrometry

  • 摘要: 建立了酱卤肉制品中同时测定1-甲基咪唑(1-methylimidazole,1-MEI)、2-甲基咪唑(2-methylimidazole,2-MEI)和4-甲基咪唑(4-methylimidazole,4-MEI)的超高效液相色谱-串联质谱(UPLC-MS/MS)的分析方法。样品经水提取,强阳离子交换固相萃取柱(Waters Oasis MCX)富集净化,氮吹复溶后,Agilent Zorbax HILIC(2.1 mm×100 mm,3.5 μm)色谱柱分离,以乙腈和5 mmol/L乙酸铵溶液为流动相梯度洗脱,采用电喷雾离子源正离子电离多反应监测模式(MRM)测定,同位素内标法定量。结果表明,1-MEI、2-MEI和4-MEI在30~400 ng/mL范围内,线性关系良好,相关系数均大于0.9997;方法检出限和定量限分别为10、30 μg/kg;在30、60、300 μg/kg加标水平下的平均回收率为92.0%~116.3%,相对标准偏差(n=6)为0.70%~3.96%。采用该方法对市售的36批次酱卤肉制品进行检测,1-MEI均未检出;2-MEI检出率为5.5%,含量为21.4~23.6 μg/kg;4-MEI检出率为100%,含量为3.1~306.6 μg/kg。该方法灵敏、快速、准确,适用于酱卤肉制品中1-MEI、2-MEI和4-MEI的定性定量测定。

     

    Abstract: An ultrahigh performance liquid chromatography-tandem mass spectorometric (HPLC-MS/MS) method was developed for the simultaneous determination of 1-methylimidazole (1-MEI), 2-methylimidazole (2-MEI) and 4-methylimidazole (4-MEI) in sauced meat products. The sample was extracted with water and the extracting solution was cleaned by Waters Oasis MCX SPEcolumn. The eluantwas dried under a stream of nitrogen and dissolved with initial mobile phase, the analytes were then separated by the Agilent Zorbax HILIC (2.1 mm×100 mm, 3.5 μm) using binary mobile phase gradient with acetonitrile and 5 mmol/L ammonium acetate. The compounds were ionized by positive electrospay, then detected under the multiple reaction monitoring (MRM) mode and quantified by the isotope internal standard method. The linearity of 1-MEI, 2-MEI and 4-MEI in the range from 30~400 ng/mL exhibited correlation coefficients greater than 0.9997. The limits of detection (LOD) and quantification (LOQ) were 10, 30 μg/kg. The average recoveries at three level spiked concentrations (30, 60, 300 μg/kg) ranged from 92.0% to 116.3%, with the relative standard deviations (n=6) between 0.70% and 3.96%. The method was applied to detect 36 sauced meat products, the 1-MEI was not detected in sauced meat products;the detection rate of 2-MEI was 5.5%, the content was 21.4~23.6 μg/kg, 4-MEI was detected in all of samples, the content was 3.1~306.6 μg/kg. The method was simple, rapid, sensitive and reliable, could be applied to determine1-MEI, 2-MEI and 4-MEI in sauced meat products.

     

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