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

中文关键词:  烷基酚聚氧乙烯醚  辛基酚聚氧乙烯醚  壬基酚聚氧乙烯醚  水果蔬菜  分散固相萃取  超高效液相色谱-串联质谱法

英文关键词:alkylphenol ethoxylates  4-octylphenol-ethoxylate  4-nonylphenol-ethoxylate  fruits and vegetables  dispersed solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      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, C18)、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2~100 μg/L的线性范围内相关系数(r)均大于0.99, 检出限分别为0.5 μg/kg和0.4 μg/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。

英文摘要:

      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 (C18) 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?100 μg/L was greater than 0.99, the limits of detection were 0.5 μg/kg and 0.4 μg/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.