首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >Simultaneous determination of carvacrol and thymol in bee pollen by using a simple and efficient solvent extraction method and gas chromatography-mass spectrometry
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Simultaneous determination of carvacrol and thymol in bee pollen by using a simple and efficient solvent extraction method and gas chromatography-mass spectrometry

机译:用简单高效的溶剂萃取方法和气相色谱 - 质谱法同时测定蜂花粉中的钙汞和胸腺酚

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摘要

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 mu g/kg), good precision (relative standard deviation values lower than 8%) and sensitivity (limits of detection and quantification lower than 15 mu g/kg). Finally, several bee pollen samples are analysed, and thymol and carvacrol residues are found at low concentrations (limit of quantification-57 mu g/kg) in some cases. (C) 2020 Elsevier B.V. All rights reserved.
机译:提出了一种新的方法,以通过偶联至质谱法通过气相色谱法测定蜂花粉中的钙汞和晶醇残留物。这是一种有效且简单的样品处理(平均分析物回收率在90%至104%之间),涉及溶剂萃取,然后蒸发。不需要任何额外的清洁步骤,因为基质没有影响大量化合物的质谱法的测定。还优化了色谱条件:采用ZB-Wax柱,氦气以1.1ml / min的流速为载气,并且包括温度程序,允许两种化合物在少于21分钟的基线分离。该方法在选择性方面完全验证,检测和定量限制,矩阵效应,线性度,精度和真实性。结果表明,它不仅选择性,而且还显示出宽的线性范围(量化-1000μg/ kg的限制),精度良好(相对标准偏差值低于8%)和灵敏度(检测和量化的限制低于15 mu g / kg)。最后,分析了几种蜂花粉样品,在某些情况下,在低浓度(定量-57μg/ kg的极限下发现胸腺酚和碳酸残基。 (c)2020 Elsevier B.v.保留所有权利。

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