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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
吴剑平,严凤,张婧,王博,潘娟,贡松松,达列亚.阿合买提
0
(上海市兽药饲料检测所)
摘要:
目的 建立超高效液相色谱-静电轨道阱质谱联用测定鸡蛋中五氯苯酚残留量的分析方法。方法 取均质后的鸡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0.22 μm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 五氯苯酚在0.5~ 100 μg/kg范围内线性关系良好(r>0.995),方法的最低检出限为0.2 μg/kg, 最低定量限为0.5 μg/kg, 添加回收率在74.43%~96.85%内,相对标准偏差(relative standard deviation, RSD)<10%。结论 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。
关键词:  五氯苯酚  分散固相萃取  静电轨道阱质谱
DOI:
投稿时间:2020-08-21修订日期:2021-04-01
基金项目:
Determination of pentachlorophenol residues in eggs by dispersive solid phase extraction combined with ultra performance liquid chromatography- orbitrap mass spectrometry
(Shanghai Municipal Supervisory Institute Veterinary Drugs and Feedstaff)
Abstract:
ABSTRACT: Objective 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. Methods 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 0.22 μm 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 Pentachlorophenol had good linear relationships in the range of 0.5- 100 μg/kg, and the correlation coefficients were above 0.995. The limit of detection of the method was 0.2 μg/kg and the minimum limit of quantitative was 0.5 μg/kg. The recovery were between 74.43% and 96.85%, with the relative standard deviation (RSD) were lower than 10%. Conclusion This method has good accuracy and precision, which is suitable for the determination of pentachlorophenol residues in eggs. KEY WORDS: pentachlorophenol; dispersive solid phase extraction; orbitrap mass
Key words:  pentachlorophenol  dispersive solid phase extraction  orbitrap mass

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