分散固相萃取-超高效液相色谱-串联质谱法测定酱油中的2-甲基咪唑和4-甲基咪唑
目的 建立测定酱油中2-甲基咪唑和4-甲基咪唑的分散固相萃取-超高效液相色谱-串联质谱(dSPE- UPLC-MS/MS)分析方法。方法 样品加入同位素内标后, 以水稀释, 并调至碱性, 用乙腈提取, 加入无水MgSO4和无水NaAC, 老抽样品再经N-丙基乙二胺(PSA)/多壁碳纳米管(MWNTs)分散净化, 采用UPLC BEH HILIC (50 mm×2.1 mm, 1.7 μm )色谱柱分离, 以乙腈-10 mmol/L乙酸铵溶液(含0.1%甲酸, v/v)为流动相等度洗脱, 采用电喷雾离子源串联质谱, 正离子多反应监测模式检测, 以同位素内标定量。结果 2-甲基咪唑和4-甲基咪唑的方法检出限均为1.5 μg/kg; 在1.0~100 μg/L浓度范围内线性关系良好, 相关系数均大于0.999; 在生抽和老抽样品中进行3个水平的添加实验, 平均回收率(n=6)为89.6%~117.2%, 日内精密度为4.8%~12.9%, 日间精密度(n=5)小于15%。结论 本方法简单快速、准确灵敏, 适用于酱油中2-甲基咪唑和4-甲基咪唑的测定。
Objective To establish a simple and rapid method for determination of 2-methylimidazole (2-MID) and 4-methylimidazole (4-MID) in soy sauce using dispersive solid phase extraction (dSPE) clean-up and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The isotope internal standard was added into the samples, which then was diluted with water and adjusted to alkaline, processed by liquid-liquid extraction with acetonitrile, followed by adding anhydrous MgSO4 and anhydrous NaAC. Then the extract of dark soy sauce was purified by primary secondary amine (PSA) sorbent plus multi-walled carbon nanotubes (MWNTs). The ultimate solution was separation with UPLC BEH HILIC (50 mm?2.1 mm, 1.7 μm), elution with acetonitrile and 10 mmol/L ammonium acetate (containing 0.1% formic acid, v/v), and detection with tandem mass spectrometry under ESI at positive and multiple reaction monitoring (MRM) mode. The targets were quantified by isotope internal standard. Results The limit of detection (LOD) of the MIDs were both 1.5 μg/kg, and the linear range were 1.0~100 μg/L with the correlation coefficients larger than 0.999. The average recoveries ranged from 89.6% to 117.2%, and within-day precisions were in a range of 4.8%~12.9% when three levels of standard were spiked into light and dark soy sauce. The inter-day precisions were less than 15%. Conclusion The developed method is simple, rapid, accurate and sensitive for the detection of 2-MID and 4-MID in soy souse.
标题：分散固相萃取-超高效液相色谱-串联质谱法测定酱油中的2-甲基咪唑和4-甲基咪唑
英文标题：Quantitative determination of 2-and 4-methylimidazole in soy sauce using dispersive solid phase extraction and ultra-high performance liquid chromatography-tandem mass spectrometry ry
作者：
吴玉銮 广州质量监督检测研究院
冼燕萍 广州质量监督检测研究院
郭新东 广州质量监督检测研究院
罗海英 广州质量监督检测研究院
王莉 广州质量监督检测研究院
韩婉清 广州质量监督检测研究院
陈立伟 广州质量监督检测研究院
李核 华南师范大学化学与环境学院
中文关键词:2-甲基咪唑,4-甲基咪唑,超高效液相色谱-串联质谱法,分散固相萃取,酱油,
英文关键词:2-methylimidazole,4-methylimidazole,ultra-high performance liquid chromatography-tandem mass spectrometry,dispersive solid phase extraction,soy souse,
发表日期：2014-04-09
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