Xiaojia Huang, Linli Chen, Dongxing Yuan.Journal

of Hazardous Materials, 2013. 262: 121-129.

In this study, a new stir cake sorptive extraction (SCSE) based

on poly(4-vinylbenzoic acid-divinylbenzene) (VBADB) monolith was prepared. The

effect of preparation conditions of monolith on extraction efficiencies was

investigated in detail. Several characteristic techniques, such as elemental

analysis, infrared spectroscopy, mercury intrusion porosimetry and scanning

electron microscopy were used to characterize the monolithic material. The

combination of SCSE-VBADB with high-performance liquid chromatography tandem

mass spectrometry (HPLC/MS/MS) detection was developed for sensitive

determination of ultra-trace β-agonists in milk and swine urine samples. In

order to obtain the optimal extraction conditions of SCSE-VBADB for β-agonists,

several extractive parameters, including pH values and ionic strength in sample

matrix, extraction and desorption time were optimized. Under the optimum

conditions, the limits of detection (S/N= 3) for the target analytes were

0.007–0.030 μg/L in milk and 0.002–0.011 μg/L in swine urine,

respectively. Excellent method reproducibility was achieved in terms of

intraday and interday precisions, indicated by the RSDs of both <10 .0%,

respectively. Finally, the proposed method was successfully used to detect

β-agonists in different milk and swine urines samples. Acceptable recoveries

ranged from 50.3% to 113% and 50.1% to 92.2% for milk and swine urine samples,

respectively; and the RSDs for reproducibility were less than 8.0% for target

analytes in all real samples.

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