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建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查和分析水产品中多种环境激素的方法。样品经乙酸乙酯提取,Captiva ND Lipids小柱净化,用C_(18)色谱柱(2.1 mm×50 mm,1.7μm)分离,以甲醇和水溶液为流动相进行梯度洗脱。采用正、负离子切换同时测定21种环境激素,大大提高检测通量。以全扫描模式下提取的保留时间和一级母离子精确质量数,实现对水产品中多种环境激素的快速筛查;以自动触发采集的二级碎片离子精确质量数进行确证。结果表明,目标化合物的线性相关系数R~2>0.99;检出限≤5μg/kg,回收率范围为71.6%~109.7%,相对标准偏差为6.0%~13%。方法适用于水产品中多种环境激素的高通快速定性筛查和定量分析。
A method of rapid screening and analysis of a variety of environmental hormones in aquatic products by ultra-high performance liquid chromatography-quadrupole / electrostatic field orbit-well high-resolution mass spectrometry was established. The sample was extracted with ethyl acetate and purified on a Captiva ND Lipids cartridge. The residue was separated on a C 18 column (2.1 mm × 50 mm, 1.7 μm) and eluted with a mobile phase of methanol and water. Using positive and negative ion switching simultaneous determination of 21 kinds of environmental hormones, greatly improving the detection flux. The rapid screening of various environmental hormones in aquatic products was achieved by using the retention times extracted in full scan mode and the exact masses of primary ions. The exact mass of secondary fragment ions collected by automatic triggering was validated. The results showed that the linear correlation coefficient of the target compounds was R ~ 2> 0.99. The detection limit was ≤5μg / kg. The recoveries ranged from 71.6% to 109.7%. The relative standard deviations were 6.0% ~ 13%. The method is suitable for high-pass rapid qualitative screening and quantitative analysis of various environmental hormones in aquatic products.