固相萃取-高效液相色谱-串联质谱法同时测定动物源性食品中五氯酚和游离棉酚

Simultaneous Determination of Pentachlorophenol and Free Gossypol in Animal-Derived Foods by Solid-Phase Extraction Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了固相萃取-高效液相色谱-串联质谱法同时测定动物源性食品中五氯酚和游离棉酚的方法。样品经乙腈-水溶液含5%三乙胺溶液(7:3,v/v)提取,采用阴离子固相萃取柱净化,经Phenomenex Knietex®F5色谱柱(100 mm×2.1 mm,2.6μm)分离,以乙腈-0.1%甲酸水为流动相,进行梯度洗脱,以电喷雾离子源负离子多反应监测(MRM)模式进行质谱检测。采用基质匹配标准曲线法定量,以降低样品基质效应的影响。结果表明:五氯酚和棉酚在各自的线性范围内线性关系良好(相关系数r^2>0.999),检出限和定量限分别在0.3~0.5μg/kg和1.0~2.0μg/kg。在低、中、高3个水平下的加标回收率在85.2%~112.6%,相对标准偏差(RSD)为1.8%~5.8%(n=6)。该方法简单、快捷、高效、准确、可靠,可用于动物源性食品中五氯酚和游离棉酚的同时快速检测。

A simple and rapid method based on solid-phase extraction and high-performance liquid chromatography-tandem mass spectrometry for the simultaneous determination of pentachlorophenol and free gossypol in animal-derived foods was developed.The target analytes in samples were extracted with acetonitrile and water containing 5%(v/v)triethylamine(7:3,v/v)and cleaned using an anion exchanging solid phase extraction column.The analytes were separated on a Phenomenex Knietex~?F5 column(100 mm×2.1 mm,2.6μm)using acetonitrile-0.1%(v/v)formic acid as a mobile phase for gradient elution,and then determined by tandem mass spectrometry in negative ESI modes under multiple reaction monitoring(MRM).The matrix matched calibration curve method was used to further suppress the matrix effect.Calibration curves were linear within a studied range of concentrations(r^2>0.999)for pentachlorophenol and free gossypol.The limits of detection(LODs)and limits of quantification(LOQs)were within 0.2~0.5μg/kg and 0.5~2μg/kg,respectively.The recoveries varied from 80.6%to 112.6%at three spiked levels,with relative standard deviations(RSDs)between 1.8%and 5.8%(n=6).The developed method is simple,rapid,efficient,accurate,reliable and is effective for the simultaneous determination of pentachlorophenol and free gossypol in animal-derived foods.