New monolithic stir-cake-sorptive extraction for the determination of polar phenols by HPLC.
A novel porous monolith has been prepared and used as a sorbent in stir-cake-sorptive extraction (SCSE). The monolithic material was prepared by in-situ copolymerization of allyl thiourea (AT) and divinylbenzene (DB) in the presence of dimethylformamide as a porogen solvent. To optimize the polymerization conditions, different monoliths with different ratios of functional monomer to porogenic solvent were prepared, and their extraction efficiency was investigated in detail. The monolith was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, and infrared spectroscopy. Analysis of polar phenols in environmental water samples by a combination of ATDB-SCSE and HPLC with diode-array detection was selected as a model for the practical application of the new sorbent. Several extraction conditions, including extraction and desorption time, pH, and ionic strength of the sample matrix were optimized. The results showed that the new monolith had high affinity for polar phenols and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the phenols, within the ranges 0.18-0.90 and 0.59-2.97 μg L(-1), respectively. The linearity of the method was good, and the method enabled simple, practical, and low-cost extraction of these analytes. The distribution coefficients between ATDB and water (K(ATDB/W)) were calculated for the phenolic compounds and compared with K(O/W). Finally, the proposed method was successfully applied to the determination of the compounds in three environmental water samples, with acceptable recovery and satisfactory repeatability.
State Key Laboratory of Marine Environmental Science, College of the Environment and Ecology, Xiamen University, P.O. Box 1009, Xiamen 361005, China. hxj@xmu.edu.cn
Xiaojia
X
Huang
Yulei
Y
Wang
Dongxing
D
Yuan
Xiaojing
X
Li
Shuyu
S
Nong
D000327:Adsorption; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D015394:Molecular Structure; D010636:Phenols / Q000737:chemistry* / Q000302:isolation & purification*; D012117:Resins, Synthetic; D052616:Solid Phase Extraction / Q000295:instrumentation / Q000379:methods*; D014874:Water Pollutants, Chemical / Q000737:chemistry* / Q000302:isolation & purification*
D010636:Phenols; D012117:Resins, Synthetic; D014874:Water Pollutants, Chemical