Tan Dongqin, Jin Jing, Li Fang, Sun Xiaoli, Ni Yuwen, Chen Jiping
Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China; University of Chinese Academy of Sciences, Beijing 100049, China.
Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, No. 457 Zhongshan Road, Dalian 116023, China.
Anal Chim Acta. 2017 Mar 1;956:14-23. doi: 10.1016/j.aca.2016.12.040. Epub 2017 Jan 2.
Magnesium oxide microspheres functionalized with phenyltrichlorosilane (PTS-MgO) were synthesized by surface modification through silanization reaction, which was confirmed by Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetry analysis (TGA) and N adsorption-desorption. The result indicated that PTS-MgO not only possessed the ability of enhancing the retention with PAHs, but also weakening the interference from chlorinated compounds. As a sorbent for the matrix solid-phase dispersion (MSPD) extraction, PTS-MgO was used to selectively extract seven dioxin-like polycyclic aromatic hydrocarbons (DL-PAHs) from soil samples. Various parameters affecting the recoveries of seven DL-PAHs were investigated and optimized, such as sorbent/sample mass ratio, grinding time, rinsing and eluting conditions. Under the optimized conditions, the developed method combining MSPD with HPLC-FLD exhibited good sensitivity (0.02-0.12 ng g detection of limits) and linearity (linear correlation coefficient greater than 0.9997). Satisfactory recoveries with DL-PAHs spiked at two levels (10 and 80 ng g) were obtained in the range of 72.2-113.1% with RSD < 9.6%, indicating that PTS-MgO had a potential in MSPD extraction of DL-PAHs in soils. Additionally, the proposed MSPD-HPLC-FLD method was also verified by detecting seven DL-PAHs in the standard reference soil. Based on the developed method, DL-PAHs in soil samples were detected with the concentration ranging from 70.08 to 555.05 ng g dry weight (dw). The total toxic equivalency quotients (TEQ) of seven DL-PAHs varied from 9.93 to 143.94 ng TEQ/g dw.
通过硅烷化反应进行表面改性合成了用苯基三氯硅烷功能化的氧化镁微球（PTS-MgO），通过傅里叶变换红外光谱（FT-IR）、扫描电子显微镜（SEM）、X射线衍射（XRD）、热重分析（TGA）和N吸附-脱附对其进行了表征。结果表明，PTS-MgO不仅具有增强对多环芳烃保留的能力，还能减弱氯代化合物的干扰。作为基质固相分散（MSPD）萃取的吸附剂，PTS-MgO用于从土壤样品中选择性萃取7种二噁英类多环芳烃（DL-PAHs）。研究并优化了影响7种DL-PAHs回收率的各种参数，如吸附剂/样品质量比、研磨时间、冲洗和洗脱条件。在优化条件下，所建立的MSPD与HPLC-FLD联用方法具有良好的灵敏度（检测限为0.02 - 0.12 ng/g）和线性（线性相关系数大于0.9997）。在两个加标水平（10和80 ng/g）下，DL-PAHs的回收率在72.2 - 113.1%范围内，相对标准偏差（RSD）< 9.6%，表明PTS-MgO在土壤中DL-PAHs的MSPD萃取方面具有潜力。此外，所提出的MSPD-HPLC-FLD方法还通过检测标准参考土壤中的7种DL-PAHs进行了验证。基于所建立的方法，检测到土壤样品中DL-PAHs的浓度范围为70.08至555.05 ng/g干重（dw）。7种DL-PAHs的总毒性当量商（TEQ）在9.93至143.94 ng TEQ/g dw之间。
