超高效液相色谱-串联四极杆质谱结合分散固相萃取技术测定禽蛋中五氯苯酚残留量

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

中文关键词:  五氯苯酚  分散固相萃取  串联四极杆质谱

英文关键词:pentachlorophenol  dispersive solid phase extraction  triple quadrupole tandem mass

中文摘要:

      目的 建立超高效液相色谱-串联四级杆质谱结合分散固相萃取技术测定禽蛋中五氯苯酚残留量的分析方法。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上层提取液, 经0.1%(V:V)甲酸溶液稀释后, 用酸性氧化铝粉末净化样品并以10000 r/min离心取上清液, 过0.22 μm滤膜后上机测定。使用流动相为乙腈: 0.1%甲酸=65:35(V:V), 采用反相色谱柱分离, 等度程序洗脱, 串联四级杆质谱法定性定量分析。结果 五氯苯酚在5~250 μg/kg范围内线性关系良好(r>0.995), 方法的检出限为2.5 μg/kg, 定量限为5 μg/kg, 添加回收率为74.44%~91.91%, 相对标准偏差(relative standard deviation, RSD)低于10%。结论 该方法具有较好的精密度与准确度, 适用于禽蛋中五氯苯酚残留量的测定。

英文摘要:

      Objective To establish a method for determination of pentachlorophenol residues in eggs by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry combined with dispersive solid phase extraction technology. Methods Homogenized egg samples were extracted with acetonitrile, and dehydrated and salted out with anhydrous magnesium sulfate and sodium chloride. After high speed centrifugation and stratification, the upper 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 detected after filtered by 0.22 μm film. The targets was separated by isocratic elution with a reverse phase column as the stationary phase and acetonitrile: 0.1% formic acid=65:35 (V:V) as the mobile phase. Triple quadrupole tandem mass spectrometry was used for qualitative and quantitative analysis. Results Pentachlorophenol had good linear relationships in the range of 5?250 μg/kg, and the correlation coefficients were above 0.995. The limit of detection of the method was 2.5 μg/kg and the limit of quantitative was 5 μg/kg. The recoveries were 74.44%?91.91%, the relative standard deviation (RSD) were lower than 10%. Conclusion This method has good precision and accuracy, which is suitable for the determination of pentachlorophenol residues in eggs.