Ares Ana M, Ayuso Irene, 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.
J Chromatogr B Analyt Technol Biomed Life Sci. 2016 Feb 15;1012-1013:130-6. doi: 10.1016/j.jchromb.2016.01.028. Epub 2016 Jan 22.
In this study, we investigate for the first time the presence of sulforaphane (SFN) residues in two of the most currently consumed food/dietary supplements, royal jelly and bee pollen. Chromatography-tandem mass spectrometry (LC-MS/MS) was the method employed, the mass spectrometer consisting of an ion-trap mass analyzer used with electrospray ionization (ESI) in positive ion mode. An efficient sample treatment involving a solvent extraction with methanol, centrifugation, and concentration in a rotary evaporator was proposed. In all cases average analyte recoveries were between 92 and 106%. Chromatographic analysis (16min) was performed on a core-shell technology based column (Kinetex C18, 150×4.6mm, 2.6μm, 100Å). The mobile phase consisted of 0.02M ammonium formate in water and acetonitrile, with a flow rate of 0.5mL/min in gradient elution mode. The fully validated method was selective, linear from 8 to 1000μg/kg (bee pollen), or from 10 to 1250μg/kg (royal jelly), precise and accurate; relative standard deviation (% RSD) and relative error (% RE) values were below 10%. Low limits of detection (LOD) and quantification (LOQ) were obtained, namely, 3μg/kg (LOD) and 8 (bee pollen) and 10 (royal jelly) μg/kg (LOQ). The method was applied for SFN analysis in several royal jelly and bee pollen samples. SFN was detected at trace levels in some bee pollen samples (<23μg/kg) examined, whilst SFN went undetected in the royal jelly samples analyzed.
在本研究中，我们首次调查了目前消费最多的两种食品/膳食补充剂——蜂王浆和蜂花粉中萝卜硫素（SFN）残留的存在情况。采用的方法是色谱 - 串联质谱法（LC-MS/MS），质谱仪由与电喷雾电离（ESI）联用的离子阱质量分析仪组成，采用正离子模式。我们提出了一种高效的样品处理方法，包括用甲醇进行溶剂萃取、离心以及在旋转蒸发器中浓缩。在所有情况下，分析物的平均回收率在92%至106%之间。色谱分析（16分钟）在基于核壳技术的色谱柱（Kinetex C18，150×4.6mm，2.6μm，100Å）上进行。流动相由水中的0.02M甲酸铵和乙腈组成，在梯度洗脱模式下流速为0.5mL/min。该经过充分验证的方法具有选择性，在8至1000μg/kg（蜂花粉）或10至1250μg/kg（蜂王浆）范围内呈线性，精密度和准确度高；相对标准偏差（%RSD）和相对误差（%RE）值均低于10%。获得了较低的检测限（LOD）和定量限（LOQ），即3μg/kg（LOD）以及8（蜂花粉）和10（蜂王浆）μg/kg（LOQ）。该方法应用于多个蜂王浆和蜂花粉样品的SFN分析。在所检测的一些蜂花粉样品中检测到痕量水平的SFN（<23μg/kg），而在所分析的蜂王浆样品中未检测到SFN。
