Ares Ana M, Valverde Silvia, Bernal José L, Nozal María J, Bernal José
IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011 Valladolid, Spain.
IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011 Valladolid, Spain.
Food Chem. 2015 Aug 15;181:263-9. doi: 10.1016/j.foodchem.2015.02.085. Epub 2015 Feb 24.
A new method was developed to determine sulforaphane (SFN) in honey using liquid chromatography tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI). An efficient extraction procedure was proposed (average analyte recoveries were between 92% and 99%); this involved a solid phase extraction (SPE) with a polymeric sorbent. Chromatography was performed on a Synergi™ Hydro analytical column with a mobile phase of 0.02 M ammonium formate in water and acetonitrile, at a flow rate of 0.5 mL/min. The method was fully validated in terms of selectivity, limits of detection (LOD) and quantification (LOQ), linearity, carry-over effect, reinjection reproducibility, precision and accuracy. The LOD and LOQ values were below 0.8 μg/kg and 2.6 μg/kg, respectively. The proposed method was applied to analyze SFN in honey from different botanical origins (rosemary, multifloral, orange blossom and heather), and SFN was detected at trace levels in some of the honey samples examined.
开发了一种使用液相色谱串联质谱法（LC-MS/MS）结合电喷雾电离（ESI）来测定蜂蜜中萝卜硫素（SFN）的新方法。提出了一种高效的提取程序（分析物平均回收率在92%至99%之间）；该程序涉及使用聚合物吸附剂的固相萃取（SPE）。在Synergi™ Hydro分析柱上进行色谱分析，流动相为水中0.02 M甲酸铵和乙腈，流速为0.5 mL/min。该方法在选择性、检测限（LOD）和定量限（LOQ）、线性、残留效应、再进样重现性、精密度和准确度方面得到了充分验证。LOD和LOQ值分别低于0.8 μg/kg和2.6 μg/kg。所提出的方法应用于分析不同植物来源（迷迭香、多花、橙花和石南花）蜂蜜中的SFN，在所检测的一些蜂蜜样品中检测到了痕量水平的SFN。
