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改良 QuEChERS-高效液相色谱-串联质谱法快速测定马铃薯和黄瓜中的乙撑硫脲

A rapid determination method for ethylenethiourea in potato and cucumber by modified QuEChERS - high performance liquid chromatography-tandem mass spectrometry.

机构信息

Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China.

出版信息

Food Chem. 2013 Jun 1;138(2-3):1355-9. doi: 10.1016/j.foodchem.2012.11.038. Epub 2012 Nov 17.

Abstract

A rapid and sensitive analytical method for the determination of ethylenethiourea (ETU) in potatoes and cucumbers is developed. This method employs modified QuEChERS followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis. ETU was extracted by alkaline acetonitrile (containing 1%NH(3).H(2)0), separated on a ZIC-pHILIC column, confirmed by multiple reaction monitoring (MRM) mode with electrospray ionisation source. This modified procedure showed satisfactory recovery (90.6-103.5%) fortified at the range of 0.005-0.05 mg kg(-1) with relative standard deviation (RSD)<7%. The limits of detection (LOD) and the limits of quantification (LOQ) were 0.002 mg kg(-1) and 0.005 mg kg(-1), respectively. Matrix effect and HILIC retention mechanism were also evaluated. The method was finally applied to detect ETU in potato and cucumber samples collected at harvest period. Residues of ETU were detected in four cucumber samples with the level lower than LOQ.

摘要

建立了一种快速、灵敏的测定马铃薯和黄瓜中乙撑硫脲(ETU)的分析方法。该方法采用改良的 QuEChERS 提取,结合高效液相色谱-串联质谱(HPLC-MS/MS)分析。碱性乙腈(含 1%NH(3).H(2)0)提取 ETU,在 ZIC-pHILIC 柱上分离,电喷雾离子源采用多反应监测(MRM)模式进行确证。改良后的方法在 0.005-0.05mg/kg 添加范围内的回收率为 90.6-103.5%,相对标准偏差(RSD)<7%。检出限(LOD)和定量限(LOQ)分别为 0.002mg/kg 和 0.005mg/kg。还评估了基质效应和 HILIC 保留机制。该方法最终应用于收获期采集的马铃薯和黄瓜样品中 ETU 的检测。在 4 个黄瓜样品中检测到 ETU 残留,其水平低于 LOQ。

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