C_(18)膜萃取-超高效液相色谱-串联质谱法测定海水中羟基多环芳烃

Determination of hydroxylated polycyclic aromatic hydrocarbons in seawater by ultra performance liquid chromatography and mass spectrometry-C_(18) membrane disk extraction

建立了C_(18)固相膜萃取-超高效液相色谱/质谱法测定海水中11种羟基多环芳烃(OHPAHs)的方法。利用C_(18)固相膜对4L海水中11种OH-PAHs进行富集,二氯甲烷超声提取,浓缩后进入C_(18)柱色谱,以乙腈-0.02%氨水为流动相梯度淋洗后进入质谱检测,11种OH-PAHs的浓度与其峰面积呈线性关系,方法检出限为0.290~2.04 ng/L,平均回收率为60.8%~96.4%,相对标准偏差均低于13%。利用本方法对河北养殖区海水中11种OH-PAHs进行检测,OH-PAHs的浓度处于1.81~10.0 ng/L之间。本法为远距离、大体积水样中痕量OH-PAHs的提取富集与测定提供了解决方案。

A new method for determining 11 hydroxyl polycyclic aromatic hydrocarbons（OH-PAHs）in seawater was established by combining the C（18） membrane disk extraction with ultra performance liquid chromatography and mass spectrometry（UPLC-MS/MS）. 11 OH-PAHs from 4 L seawater were enriched by C（18） membrane, and then ultrasonic extracted by dichloromethane. After being concentrated,compounds were separated by C（18） column and were detected by mass spectrometry with CH3 CN/NH3·H2 O（0. 2%） as mobile phase gradient elution. The peak areas of 11 OH-PAHs were linearly dependent with their concentrations and the detection limit were 0. 290 ~ 2. 04 ng/L. The average recoveries were 60. 8% ~ 96. 4% and the relative standard deviations were less than 13%.This method was applied to analyze the concentration of 11 OH-PAHs in the seawater of Hebei aquaculture area,and the results showed that the concentration of OH-PAHs was 1. 81 ~ 10. 0 ng/L.The method is applicable to determine the concentration of OH-PAHs in large volume of water samples.