分散固相萃取净化-超高效液相色谱-串联质谱法测定水果蔬菜中烷基酚聚氧乙烯醚

Determination of alkylphenol ethoxylates in fruits and vegetables by dispersive solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

目的建立分散固相萃取净化-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)快速测定水果蔬菜中壬基酚聚氧乙烯醚[4-nonylphenol-ethoxylate,NP(EO)_(3~17)]和辛基酚聚氧乙烯醚[4-octylphenol-ethoxylate,OP(EO)_(3~17)]残留量的检测方法。方法样品经乙腈:丙酮(8:2,V:V)超声提取,提取液使用混合吸附剂[多壁碳纳米管(multi-walled carbon nano-tube,MWCNTs)、十八烷基硅烷键合硅胶(octadecylsilane,C_(18))、N-丙基乙二胺(primary secondary amine,PSA)]净化,净化后样液通过Phenomenex Kinetex Biphenyl色谱柱分离,乙腈-10 mmol/L乙酸铵溶液梯度洗脱,在单离子检测扫描(single ion monitoring,SIM)模式下进行定性和定量分析。结果NP(EO)_(3~17)和OP(EO)_(3~17)在2~100μg/L的线性范围内相关系数(r)均大于0.99,检出限分别为0.5μg/kg和0.4μg/kg,回收率为74.5%~109.2%,相对标准偏差为2.5%~14.9%。结论该方法简单、快捷、稳定、灵敏度高,可用于水果蔬菜中NP(EO)_(3~17)和OP(EO)_(3~17)的快速筛查。

Objective To establish a method for the rapid determination of 4-nonylphenol-ethoxylate[NP(EO)_(3~17)]and 4-octylphenol-ethoxylate[OP(EO)_(3~17)]in fruits and vegetables by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)based on dispersive solid phase extraction pre-treatment technology.Methods The samples were extracted with acetonitrile:acetone(8:2,V:V)in ultrasonic way,and the extraction solution was purified by mixed purifying material[multi-walled carbon nano-tube(MWCNTs),octadecylsilane(C_(18))and primary secondary amine(PSA)].After purification,the samples were separated by Phenomenex Kinetex Biphenyl column,eluted with acetonitrile-10 mmol/L ammonium acetate solution as mobile phase,and analyzed qualitatively and quantitatively in single ion monitoring(SIM)mode.Results The correlation coefficient(r)of NP(EO)_(3~17) and OP(EO)_(3~17) in the linear range of 2‒100μg/L was greater than 0.99,the limits of detection were 0.5μg/kg and 0.4μg/kg,respectively,the recoveries of method were 74.5%‒109.2%,and the relative standard deviations were 2.5%‒14.9%.Conclusion This method is simple,rapid,stable,sensitive.It’s suitable for the rapid screening of NP(EO)_(3~17) and OP(EO)_(3~17) in fruits and vegetables.