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目的建立超高效液相色谱-高分辨质谱法检测调味品中19种非食用物质的分析方法。方法样品经乙酸乙酯-环己烷提取,采用凝胶渗透色谱(gel permeation chromatography,GPC)净化与在线定量浓缩,然后经C_(18)色谱柱分离,乙腈和5 mmol/L乙酸铵(含0.1%甲酸)溶液梯度洗脱后经超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry,UPLC-LTQ-orbitrap MS)测定。结果 19种目标物在15 min内实现良好分离,线性相关系数均≥0.996,定量限(limit of quantitation,LOQ)为5~15μg/kg,加标回收率在61.9%~105.8%之间,相对标准偏差(relative standard deviation,RSD)为2.3%~12.9%。结论本研究建立的方法准确、简单,可适用于调味品中19种非食用物质的定性定量及确证分析。
Objective To establish a method for the determination of 19 non-food substances in condiments by ultra performance liquid chromatography-high resolution mass spectrometry. Methods The sample was extracted with ethyl acetate - cyclohexane, purified by gel permeation chromatography (GPC) and quantified on - line quantitatively. The residue was separated on a C 18 column with acetonitrile and 5 mmol / L ammonium acetate 0.1% formic acid) and then analyzed by ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry (UPLC-LTQ-orbitrap MS) Determination. Results Nineteen target species were well separated within 15 min with linear correlation coefficients ≥0.996, limit of quantitation (LOQ) of 5-15 μg / kg and spike recoveries of 61.9% -105.8% The relative standard deviation (RSD) was 2.3% ~ 12.9%. Conclusion The method established in this study is accurate and simple, and can be applied to qualitative and quantitative analysis of 19 kinds of non-food substances in condiments.