鱼肉中五氯酚残留的测定方法建立——EMR固相萃取-超高效液相色谱-质谱法

Determination of Pentachlorophenol Residues in Fish Meat-EMR Solid Phase Extraction-High-Performance Liquid Chromatography-Mass Spectrometry

目的:建立EMR固相萃取结合超高效液相色谱-串联质谱测定鱼肉样品中五氯酚残留的分析方法。方法:经含3%甲酸的乙腈溶液提取后的鱼肉样品,被Captiva EMR-Lipid固相萃取小柱净化后,采用ACQUITY UPLC BEH C_(18)(1.7μm,100 mm×2.1 mm)色谱柱分离,电喷雾离子源负离子模式扫描,多反应监测模式,以外标法定量。结果:经EMR固相萃取净化的鱼肉样品中的五氯酚残留量在1μg/kg~50μg/kg内线性关系良好,相关系数(R^(2))均大于0.99,方法检出限(S/N=3)和定量限(S/N=10)分别为0.2μg/kg和0.5μg/kg,平均回收率在81.7%~94.2%之间,相对标准偏差(RSD)为1.5%~7.1%(n=6)。结论:本方法操作快速简单,重复性好,灵敏度较高,适用于鱼肉中五氯酚残留的检测。

objective:To develop a method for the determination of pentachlorophenol residues in fish samples by EMR solid phase extraction coupled with High-performance liquid chromatography tandem mass spectrometry.Methods:The fish meat samples were extracted with acetonitrile solution containing 3%formic acid and purified by a Captiva EMR Lipid solid-phase extraction column.The chromatographic column was ACQUITY UPLC BEH C_(18)(1.7μm,100 mm×2.1 mm)chromatographic column,electro spray ion source anion scanning,multi reaction monitoring mode and the quantitative method was external standard.Results:The residual content of pentachlorophenol in fish meat samples purified by EMR solid-phase extraction is within the range of 1μg/kg~50μg/kg and the linear relationship was good(correlation coefficient R^(2)>0.99).The limit of detection(S/N=3)and quantification(S/N=10)was 0.2μg/kg and 0.5μg/kg respectively.The average recovery rate is 81.7%~94.2%,with a relative standard deviation(RSD)of 1.5%~7.1%(n=6).Conclusions:This method is fast and simple to operate,with good repeatability and high sensitivity,and is suitable for the detection of pentachlorophenol residues in fish meat.