Cai Ying, Yan Zhihong, Wang Lijia, NguyenVan Manh, Cai Qingyun
State Key Laboratory of Chemo/Biosensing & Chemometrics, College of Chemistry & Chemical Engineering, Hunan University, Changsha 410082, China.
Key Laboratory of Modern Preparation of TCM, Ministry of Education, Jiangxi University of Traditional Chinese Medicine, Nanchang 330004, China.
J Chromatogr A. 2016 Jan 15;1429:97-106. doi: 10.1016/j.chroma.2015.12.032. Epub 2015 Dec 14.
A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples.
已开发出一种结合静态顶空气相色谱-质谱联用（HS-GC-MS）方法的磁性固相萃取（MSPE）方案，用于饮用水样品中16种多环芳烃（PAHs）的萃取和测定。磁性纳米颗粒（MNPs）用3-氨丙基三乙氧基硅烷包覆，并通过氯甲酸胆固醇酯进行改性。使用透射电子显微镜、振动样品磁强计、傅里叶变换红外光谱和X射线光电子能谱对胆固醇功能化吸附剂进行表征，并研究和确定了影响萃取以及HS采样的主要参数，如吸附剂用量、萃取时间、炉温和平衡时间。与HS采样相结合，MSPE程序简单、快速且环保，无需任何有机溶剂。方法验证证明了所开发的吸附剂用于痕量水平所研究分析物定量的可行性，检测限（S/N=3）范围为0.20至7.8 ng/L。获得了良好的日内和日间精密度值（RSDs≤9.9%）。所提出的方法成功应用于饮用水样品。
