Preparation of stir cake sorptive extraction based on poly(4-vinylbenzoic acid-divinylbenzene) monolith and its application in sensitive determination of β-agonists in milk and swine urine samples

Abstract

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 0.007–0.030μg/L in milk and 0.002–0.011μg/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.