I. U. CINQUIMA, Analytical Chemistry Group, Faculty of Sciences, University of Valladolid, Paseo De Belén 5, 47011, Valladolid, Spain.
I. U. CINQUIMA, Analytical Chemistry Group, Faculty of Sciences, University of Valladolid, Paseo De Belén 5, 47011, Valladolid, Spain.
J Pharm Biomed Anal. 2020 Mar 20;181:113124. doi: 10.1016/j.jpba.2020.113124. Epub 2020 Jan 23.
A novel method is proposed to determine residues of carvacrol and thymol in bee pollen by means of gas chromatography coupled to mass spectrometry. This is an efficient and simple sample treatment (with average analyte recoveries between 90% and 104%) involving solvent extraction with hexane followed by evaporation. There is no need for any additional clean-up step, as the matrix did not affect determination of mass spectrometry for either compound. The chromatographic conditions are also optimized: a ZB-WAX column is employed, helium is the carrier gas at a flow rate of 1.1 mL/min, and a temperature program is included, allowing baseline separation of both compounds in less than 21 min. The method is fully validated in terms of selectivity, limits of detection and quantification, matrix effect, linearity, precision and trueness. Results show that not only is it selective, but that it also displays a wide linearity range (limit of quantification-1000 μg/kg), good precision (relative standard deviation values lower than 8%) and sensitivity (limits of detection and quantification lower than 15 μg/kg). Finally, several bee pollen samples are analysed, and thymol and carvacrol residues are found at low concentrations (limit of quantification-57 μg/kg) in some cases.
提出了一种通过气相色谱-质谱联用测定蜂花粉中香芹酚和百里酚残留量的新方法。这是一种高效、简单的样品处理方法(平均分析物回收率在 90%至 104%之间),涉及用正己烷溶剂萃取,然后蒸发。由于基质对两种化合物的质谱测定均无影响,因此无需进行任何额外的净化步骤。还优化了色谱条件:采用 ZB-WAX 柱,载气为氦气,流速为 1.1 mL/min,并包括一个温度程序,使两种化合物在不到 21 min 的时间内实现基线分离。该方法在选择性、检测限和定量限、基质效应、线性、精密度和准确度方面均得到了充分验证。结果表明,该方法不仅具有选择性,而且还具有较宽的线性范围(定量限-1000 μg/kg)、良好的精密度(相对标准偏差值低于 8%)和灵敏度(检测限和定量限低于 15 μg/kg)。最后,对几个蜂花粉样品进行了分析,在某些情况下发现了低浓度的百里酚和香芹酚残留(定量限-57 μg/kg)。