柱前衍生-超高效液相色谱-串联四极杆质谱法测定茶叶中乙撑硫脲的残留

doi:10.3724/SP.J.1123.2018.08003

摘要/Abstract

摘要：

建立了茶叶中乙撑硫脲残留的柱前衍生-超高效液相色谱-串联四极杆质谱检测方法。样品采用乙腈提取，提取液经QuEChERS基质分散固相萃取净化后采用9-芴基甲基氯甲酸酯（FMOC-CL）柱前衍生；衍生溶液经BEH-C18色谱柱（100 mm×2.0 mm，1.7 μm）分离后进入串联四极杆质谱仪检测，采用同位素内标法定量；流动相为0.1%（v/v）甲酸-乙腈。该方法对茶叶样品检出限为1.3 μg/kg，定量限为4.2 μg/kg；加标回收率在97.7%~107.5%之间，相对标准偏差（RSD，n=6）在2.1%~10.0%之间；在1.0~203.4 μg/L范围内线性回归系数r为0.9993。该方法灵敏度高，重现性好，定性定量准确，可有效满足对茶叶中乙撑硫脲残留检测的要求。

关键词: 茶叶, 超高效液相色谱-串联四极杆质谱(UPLC-MS/MS), 乙撑硫脲, 柱前衍生

Abstract:

A method based on precolumn derivatization along with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of ethylenethiourea residues in tea. The sample was extracted using acetonitrile; the extracting solution was purified by matrix-dispersed solid phase extraction and precolumn derivatization using 9-fluorenylmethyl chloroformate (FMOC-CL). The UPLC separation was carried out on an Acquity BEH C18 column (100 mm×2.1 mm, 1.7 μm) and quantified using the isotope internal standard method. The mobile phase was 0.1% (v/v) formic acid and acetonitrile. For tea samples, the detection limit of this method was 1.3 μg/kg and the limit of quantitation was 4.2 μg/kg. The recoveries were in the range 97.7%-107.5% with relative standard deviation (RSD) of 2.1%-10.0% (n=6). The linear correlation coefficient (r) was 0.9993 over the concentration range 1.0-203.4 μg/L. This method showed high sensitivity, good reproducibility, and qualitative and quantitative accuracy, and could be suitable for the detection of ethylenethiourea residues in tea.

Key words: ethylenethiourea (ETU), precolumn derivatization, tea, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

郑小严. 柱前衍生-超高效液相色谱-串联四极杆质谱法测定茶叶中乙撑硫脲的残留[J]. 色谱, 2018, 36(12): 1238-1244.

ZHENG Xiaoyan. Determination of ethylenethiourea residues in tea using precolumn derivatization with ultra-performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(12): 1238-1244.

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