分散固相萃取结合UPLC-Orbitrap MS联用测定鸡蛋中五氯苯酚残留量

建立了超高效液相色谱-静电轨道阱质谱联用测定禽蛋中五氯苯酚残留量的分析方法。取均质后的禽蛋样品经乙腈溶液提取,加入无水硫酸镁和氯化钠进行脱水和盐析,高速离心分层后,取适量乙腈层溶液经0.1%(V∶V)甲酸稀释后,用酸性氧化铝粉末进行样品净化并以10000 r/min离心取上清液,过0.22μm滤膜后上机测定。使用反相色谱柱进行分离,流动相为乙腈:0.1%甲酸=75∶25,采用等度程序进行洗脱,静电轨道阱质谱进行定性定量分析。结果表明,五氯苯酚在0.5~100μg/kg范围内线性关系良好(r>0.995),方法的最低检出限为0.2μg/kg,最低定量限为0.5μg/kg,添加回收率在74.43%~96.85%之间,批内批间变异系数CV%<10%。该方法具有较好的准确度与精密度,适用于禽蛋中五氯苯酚残留量的测定。

Determination of pentachlorophenol residues in eggs by dispersive solid phase extraction combined with ultra performance liquid chromatography- orbitrap mass spectrometry

To establish a method for determination of pentachlorophenol residues in eggs by dispersive solid phase extraction combined with ultra performance liquid chromatography-orbitrap mass spectrometry,homogenized egg samples were extracted with acetonitrile,and dehydrated and salted out with anhydrous magnesium sulfate and sodium chloride.After high speed centrifugation,the extract was diluted by the 0.1%(V∶V)formic acid and purified by the acid alumina powder.After 10000 r/min centrifugation,the extract was filtered by 0.22μm film and then detected.The targets was separated by isocratic elution with a reverse phase column as the stationary phase and acetonitrile:0.1%formic acid=75∶25 as the mobile phase.Orbitrap mass spectrometry was used for qualitative and quantitative analysis.Results showed that pentachlorophenol had good linear relationships in the range of 0.5~100μg/kg,and the correlation coefficients were above 0.995.The limit of detection of the method was 0.2μg/kg and the minimum limit of quantitative was 0.5μg/kg.The recovery were between 74.43%and 96.85%,Coefficient of variation(CV%)in-batch and between-batch were lower than 10%.This method has good accuracy and precision,which is suitable for the determination of pentachlorophenol residues in eggs.