QuEChERS-气相色谱-串联质谱法快速检测茶叶中6种禁用香精成分
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摘要
建立了QuEChERS净化作为样品前处理,结合气相色谱-串联质谱(GC-MS/MS)同时检测茶叶中6种禁用香精成分(香豆素、侧柏酮、2-己基噻吩、反式-β-金合欢烯、p-薄荷-1,8(10)-二烯-9-乙酸乙酯和肉桂酸丁酯)的分析方法。茶叶样品用乙酸乙酯溶液萃取,涡旋振荡,离心后上清液中加入无水硫酸镁、十八烷基键合硅胶(C18)和乙二胺-N-丙基甲硅烷(PSA),涡旋,低温离心后过滤膜,以DB-5MS色谱柱分离,MS/MS于MRM模式下测定,基质曲线外标法定量。实验结果表明,6种禁用香精成分在1～200μg/L线性范围内呈良好线性,线性相关系数(R~2)均大于0.999。方法检出限0.005～1μg/kg,定量限0.02～2μg/kg,平均回收率82.3%～93.1%,日内、日间精密度均小于10%。该方法处理简单、快速,准确度和灵敏度高,可用于茶叶中6种禁用香精成分的检测。
QuEChERS purification was established as a sample pretreatment method and combined with gas chromatography-tandem mass spectrometry(GC-MS/MS) for the simultaneous detection of six banned fragrance components in tea(coumarin, thujone, 2-exylthiophene, trans-beta-acacene, p-mentha-1,8(10)diene-9-ethyl acetate, and butyl cinnamate). Tea samples were extracted with ethyl acetate and subjected to whirlpool oscillation, following which anhydrous magnesium sulfate, primary secondary amine(PSA), and octadecylsilyl silica gel(C18) were added to the supernatant. After centrifugation, the supernatant was filtered over a membrane and separated on a DB-5 MS column. The six compounds were determined by GC-MS/MS in MRM mode, and quantified by a matrix-matched external standard method. The six banned flavor compounds exhibited good linearity over the range of 1-200 μg/L, and the linear correlation coefficients(R~2) were greater than 0.999. The limits of detection were 0.005-1 μg/kg and the limits of quantification were 0.02-2 μg/kg, the average recoveries were 82.3%-93.1%, and the intra-day and inter-day RSDs were each less than 10%. The method is simple, rapid, accurate, and sensitive, and can be used for the simultaneous detection of six banned fragrance components in tea.
QuEChERS purification was established as a sample pretreatment method and combined with gas chromatography-tandem mass spectrometry(GC-MS/MS) for the simultaneous detection of six banned fragrance components in tea(coumarin, thujone, 2-exylthiophene, trans-beta-acacene, p-mentha-1,8(10)diene-9-ethyl acetate, and butyl cinnamate). Tea samples were extracted with ethyl acetate and subjected to whirlpool oscillation, following which anhydrous magnesium sulfate, primary secondary amine(PSA), and octadecylsilyl silica gel(C18) were added to the supernatant. After centrifugation, the supernatant was filtered over a membrane and separated on a DB-5 MS column. The six compounds were determined by GC-MS/MS in MRM mode, and quantified by a matrix-matched external standard method. The six banned flavor compounds exhibited good linearity over the range of 1-200 μg/L, and the linear correlation coefficients(R~2) were greater than 0.999. The limits of detection were 0.005-1 μg/kg and the limits of quantification were 0.02-2 μg/kg, the average recoveries were 82.3%-93.1%, and the intra-day and inter-day RSDs were each less than 10%. The method is simple, rapid, accurate, and sensitive, and can be used for the simultaneous detection of six banned fragrance components in tea.
引文
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