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目的建立超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法同时快速筛查和分析水产品中14种邻苯二甲酸酯以及3种酚类(壬基酚、辛基酚和双酚A)环境雌激素的分析方法。方法样品经乙腈提取后,经Silica/PSA固相萃取小柱净化,用ACQUITY UPLC@BENC_(18)色谱柱(2.1 mm×50 mm,1.7μm)分离,以甲醇和0.01%氨水为流动相进行梯度洗脱,采用静电场轨道阱高分辨质谱正负子切换FullMS/ddMS~2扫描方式同时测定17种环境雌激素。以保留时间和全扫描获得的化合物的精确质量数,实现对目标物的快速筛查;以自动触发采集的二级质谱图进行定性确证。结果 17种化合物的精确质量数相对质量偏差小于5×10~(-6);线性良好,相关系数(r~2)大于0.99;该方法的检出限≤5μg/kg,回收率为70.6%~114.3%,相对标准偏差(relative standard deviations,RSDs)为5.5%~14.3%。结论该方法适用于水产品中多种环境雌激素的高通量快速筛查和定量分析。
OBJECTIVE To establish simultaneous determination of 14 kinds of phthalates in aquatic products and three kinds of phenols (nonylphenol, octylphenol and octylphenol) by ultra-high performance liquid chromatography-quadrupole / electrostatic field orbithole high resolution mass spectrometry And bisphenol A) method of environmental estrogen analysis. Methods The samples were extracted with acetonitrile and purified by Silica / PSA solid phase extraction cartridges. The samples were separated on an ACQUITY UPLC @ BENC 18 column (2.1 mm × 50 mm, 1.7 μm) using methanol and 0.01% aqueous ammonia as the mobile phase Gradient elution, 17 kinds of environmental estrogens were determined simultaneously by FullMS / ddMS ~ 2 scanning mode using electrostatic field orbit well high resolution mass spectrometry. The accurate mass of the compound obtained with retention time and full scan was used to achieve rapid screening of the target. Qualitative confirmation was made by automatically triggering the acquired secondary spectrum. Results The relative mass deviation of the 17 compounds was less than 5 × 10 -6. The linearity was good and the correlation coefficient (r 2) was greater than 0.99. The detection limit of this method was less than 5 μg / kg and the recovery was 70.6% ~ 114.3%, relative standard deviations (RSDs) of 5.5% ~ 14.3%. Conclusion This method is suitable for rapid screening and quantitative analysis of a variety of environmental estrogens in aquatic products.