同位素稀释超高效液相色谱-串联质谱法同步快速测定热加工肉类中7种杂环胺

Synchronous and rapid determination of 7 kinds of heterocyclic aromatic amines in thermal processing meat by isotope dilution ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  同位素稀释  固相萃取  杂环胺  热加工肉类

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  isotope dilution  solid phase extraction  heterocyclic aromatic amines  thermal processing meat

中文摘要:

      目的 建立同位素稀释超高效液相色谱-串联质谱法同步快速测定热加工肉类中7种杂环胺含量的分析方法。方法 样品经甲醇水溶液(3:7, V:V)均质提取, 低温高速离心后上清液采用聚苯乙烯-二乙烯苯固相萃取净化。经ACQUITY UPLC?BEH C18 (150 mm×3.0 mm, 1.7 μm)反相色谱柱分离, 三重四极杆串联质谱仪在可编程多反应监测正离子模式下同位素内标法定量测定。结果 在质量浓度0.1~100.0 ng/mL范围内, 各杂环胺标准品均呈现良好线性关系, 相关系数(r2)均大于0.999, 检出限和定量限范围分别在0.02~0.04 ng/g和0.06~0.14 ng/g之间。在低、中、高3种当量水平下加标回收率范围为84.62%~111.97%, 日内精密度和日间精密度范围分别为0.83%~6.17% (n=6)和1.84%~9.78% (n=18)。结论 本方法稳定、灵敏、高效, 适用于不同热加工肉类中多种杂环胺的日常痕量检测分析。

英文摘要:

      Objective To develop an rapid method for simultaneously analyzing 7 kinds of heterocyclic aromatic amines in thermal processing meat foods based on isotope dilution ultra performance liquid chromatography-tandem mass spectrometry. Methods Homogenized samples were extracted with methanol-water solution (3:7, V:V), then the supernatant was centrifuged at low-temperature and high-speed, and cleaned up with polystyrene-divinylbenzene solid phase extraction column. The samples were separated on an ACQUITY UPLC? BEH C18 (150 mm×3.0 mm, 1.7 μm) reversed phase column, and detected by scheduled multiple reaction monitoring using triple quadrupole tandem mass spectrometer and quantified by isotope internal standard method. Results All standard solution of heterocyclic aromatic amines showed good linearity between the mass concentration of 0.1?100.0 ng/mL with high significant correlations (r2>0.999), and the limits of detection and limits of quantitation were 0.02?0.04 ng/g and 0.06?0.14 ng/g, respectively. In addition, the spiked (low, medium and high) recoveries were 84.62%?111.97%, and intra-day precisions and inter-day precisions were 0.83%?6.17% (n=6) and 1.84%?9.78% (n=18), respectively. Conclusion The method is stable, sensitive and efficient, and suitable for the daily trace analysis of various heterocyclic aromatic amines in different thermal processing meat foods.