蛋及蛋制品中五氯酚残留量的检测及其确证方法的研究

Valid Detection of Pentachlorophenol Residues in Eggs and Egg Products

建立了Oasis PRiME HLB(Hydrophilic lipophilic balance)固相萃取结合液相色谱-串联质谱分析技术测定蛋及蛋制品中的五氯酚残留量的方法。蛋及蛋制品采用90%乙腈水溶液(含8%三乙胺)充分提取后,使用Oasis PRiME HLB固相萃取小柱净化,以Agilent Eclipse Plus C18(2.1 mm×50 mm,1.8μm)作为色谱柱,甲醇-5 mmol/L乙酸铵溶液为流动相,梯度洗脱。电喷雾离子源负离子模式,多反应监测进行检测。同时采用高效液相色谱串联-四极杆飞行时间质谱联用仪开发蛋及蛋制品中五氯酚残留量检测的确证方法。结果表明,五氯酚在1.0~25.0 ng/mL范围内具有良好的线性关系,相关系数均大于0.990,各加标水平下5种基质中的平均回收率范围为85.8%~94.1%,相对标准偏差小于5.4%。该方法前处理简单快速、定量准确,能较好地检测蛋及蛋制品中五氯酚的残留量,可满足五氯酚残留情况的筛查和确证的要求。

A method was established for the determination of pentachlorophenol residues in eggs and egg products by Oasis PRiME HLB(Hydrophilic lipophilic balance)solid-phase extraction combined with liquid chromatography-tandem mass spectrometry(LC-MS/MS).After thorough extraction of eggs and egg products with a 90%acetonitrile aqueous solution containing 8%triethylamine,Oasis PRiME HLB solid-phase extraction columns were used for purification.the Agilent Eclipse Plus C_(18)(2.1 mm×50 mm,1.8μm)was used as the chromatographic column,with methanol-5 mmol/L ammonium acetate solution as the mobile phase,and a gradient elution process was employed.Electrospray ionization source was operated in negative ion mode,and multiple reaction monitoring(MRM)was utilized for detection.Simultaneously using liquid chromatography/quadrupole time-of-flight(LC/Q-TOF)to establish a confirmation method of pentachlorophenol residues in eggs and egg products.Results showed that there was a good linear ralationship for pentachlorophenol in the range of 1.0–25.0 ng/mL,and the linear correlation coefficients was above 0.990.The average recoveries rates in five matrices ranged from 85.8%to 94.1%at each spiked level,with relative standard deviations less than 5.4%.The method is simple,quick,accurate,and is suitable for the determination of pentachlorophenol residues in eggs and egg products,meeting the requirements for screening and confirming the residues of pentachlorophenol.