凝胶渗透色谱净化-超高效液相色谱串联质谱测定鱼中8种酚类内分泌干扰物的方法研究

Simutanious detection of 8 phenolic endocrine disruptors in fish by gel permeation chromatography purification extraction and ultra performance liquid chromatography mass spectrometry

目的建立同时测定鱼中双酚A(BPA)、双酚B(BPB)、双酚F(BPF)、双酚S(BPS)、正壬基酚(4-n-NP)、对壬基酚(4-NP)、4-正辛基酚(4-OP)和4-特辛基酚(4-t-OP)8种常见的酚类内分泌干扰物的方法。方法样本经乙酸乙酯-环己烷提取,凝胶渗透色谱(Biobead SX-3(300 mm×10 mm)凝胶色谱柱,乙酸乙酯-环己烷(1∶1)为流动相净化,超高效液相色谱串联质谱定性和定量。结果 8种酚类内分泌干扰物在0.1μg/L～40μg/L范围内线性关系良好(r>0.990),检出限为0.48 ng/kg～6.4 ng/kg,平均回收率为70.2%～112.1%,RSD在4.3%～13.2%。结论凝胶渗透色谱净化-超高效液相色谱串联质谱法处理操作简单,灵敏度高,可满足分析方法学的要求,可用于鱼中8种酚类内分泌干扰物的测定。

Objective To develop a method which can simutaniously detect 8 common phenolic endocrine disruptors including bisphenol A(BPA), bisphenol B(BPB), bisphenol F(BPF), bisphenol S(BPS), nonylphenol(4-n-NP), nonylphenol(4-NP), 4-octyl phenol(4-OP) and 4-polyoctyl phenol(4-t-OP) in fish. Methods The fish samples were extracted by mixtures of ethyl acetate and cyclohexane and were purified by gel permeation chromatography with Biobead SX-3(300 mm×10 mm) gel column with a mixture of ethyl acetate and cyclohexane at 1∶1 ratio as mobile phase.Qualitative and quantitative analysis was performed using ultra-high performance liquid chromatography tandem mass spectrometry. Results The 8 phenolic endocrine disruptors had a good linear relationship(r>0.990) in the range of 0.1 μg/L-40 μg/L.The detection limit ranged from 0.48 ng/kg to 6.4 ng/kg, the average recovery rate was from 70.2% to 112.1%(n=6), and RSD was between 4.3% and 13.2%. Conclusions This method is simple and sensitive, and can meet the requirements of analytical methodology.It can be used for the simutanious detection of 8 phenolic endocrine disruptors in fish.