Yao Zhijian, Zhao Qingqing, Ma Yan, Wang Wei, Zhou Qing, Li Aimin
State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing, 210023, P.R. China.
Sci Rep. 2017 Aug 14;7(1):8069. doi: 10.1038/s41598-017-08778-1.
In this research a new magnetic material called M88 was fully synthetized and characterized for the extraction of pharmaceutical and personal care products in water samples. In addition, a portable prototype of magnetic solidphase extraction (MSPE) device was developed for the onsite preconcentration. The MSPE coupling with high performance liquid chromatography-Diode array detector (HPLC-DAD) method was developed and validated for simultaneous analysis of 11 PPCPs (mefenamic acid, chloroamphenicol, ketoprofen, clofibric acid, indometacin, acetylsalicylic acid, bisphenol A, phenylphenol, gemfibrozil, triclosan, and ibuprofen) in environmental water samples. Experimental parameters affecting the extraction efficiencies, such as the amount of M88, desorption solvent, extraction time, and solution pH and sample volume were investigated. Under the optimal conditions, the limits of detection (LODs, S/N = 3) for the selected PPCPs were found to be in the range of 0.7-9.4 ng/L, with good linear correlation coefficients. It is also shown that the extraction efficiency of M88 was comparable to that of the commercial Oasis HLB and was evidently higher than that of the C18 cartridge. The optimised method was further verified by performing spiking experiments in water samples from Taihu Lake, with good recovery and reproducibility for all the compounds.
在本研究中，一种名为M88的新型磁性材料被完全合成并表征，用于从水样中萃取药物和个人护理产品。此外，还开发了一种用于现场预浓缩的磁性固相萃取（MSPE）装置便携式原型。建立了MSPE与高效液相色谱-二极管阵列检测器（HPLC-DAD）联用的方法，并对环境水样中的11种药物和个人护理产品（甲芬那酸、氯霉素、酮洛芬、氯贝酸、吲哚美辛、乙酰水杨酸、双酚A、苯酚、吉非贝齐、三氯生和布洛芬）进行了同时分析方法验证。研究了影响萃取效率的实验参数，如M88的用量、解吸溶剂、萃取时间、溶液pH值和样品体积。在最佳条件下，所选药物和个人护理产品的检测限（LOD，S/N = 3）在0.7-9.4 ng/L范围内，线性相关系数良好。研究还表明，M88的萃取效率与市售的Oasis HLB相当，明显高于C18柱。通过对太湖水样进行加标实验，进一步验证了优化后的方法，所有化合物的回收率和重现性良好。
