Laboratory for Food Safety, French Agency for Food, Environmental and Occupational Health & Safety (ANSES), Université Paris-Est, ANSES, 94700, Maisons-Alfort, France.
Department of Chemistry, Alexandru Ioan Cuza University of Iasi, Carol I Blvd., No. 11, 700506, Iasi, Romania.
Anal Bioanal Chem. 2024 Jan;416(2):431-438. doi: 10.1007/s00216-023-05034-6. Epub 2023 Nov 20.
This study reports a novel analytical approach for the simultaneous determination of ethylene-thiourea (ETU) and propylene-thiourea (PTU) in fruits and vegetables by (reverse phase) high-performance liquid chromatography (HPLC) coupled to inductively coupled plasma-tandem mass spectrometry (ICP-QQQMS or ICP-MS/MS). A baseline separation of ETU and PTU was achieved in less than 5 min. A robust method validation by using the accuracy profile approach was performed by carrying out four measurement series in duplicate at six different levels over a timespan of 4 weeks (different days). The recovery factors ranged from 87 to 101% for ETU and from 98 to 99% for PTU (depending on the spiking level). The coefficient of variation in terms of repeatability (CV) ranged from 1 to 4.7% for ETU and from 1.8 to 3.9% for PTU (depending also on the analyte level) while the coefficient of variation in terms of intermediate reproducibility (CV) ranged from 3.4 to 10% for ETU and from 1.8 to 10.8% for PTU. The limit of quantification was 0.022 mg kg (wet weight) for ETU and 0.010 mg kg (ww) for PTU. This novel approach was proved to be highly robust and suitable for the determination of ETU and PTU in foodstuffs of vegetal origin.
本研究报告了一种通过(反相)高效液相色谱(HPLC)与电感耦合等离子体质谱串联(ICP-QQQMS 或 ICP-MS/MS)联用同时测定水果和蔬菜中乙撑硫脲(ETU)和丙撑硫脲(PTU)的新分析方法。ETU 和 PTU 在不到 5 分钟的时间内实现了基线分离。通过在 4 周的时间跨度内(不同的日子)以 6 个不同水平进行 4 次重复测量系列,使用准确度概况方法进行了稳健的方法验证。ETU 的回收率范围为 87%至 101%,PTU 的回收率范围为 98%至 99%(取决于加标水平)。ETU 的重复性(CV)系数范围为 1%至 4.7%,PTU 的重复性(CV)系数范围为 1.8%至 3.9%(也取决于分析物水平),而 ETU 的中间重现性(CV)系数范围为 3.4%至 10%,PTU 的中间重现性(CV)系数范围为 1.8%至 10.8%。ETU 的定量限为 0.022 毫克/千克(湿重),PTU 的定量限为 0.010 毫克/千克(ww)。该新方法被证明具有高度的稳健性,适用于测定植物源性食品中的 ETU 和 PTU。