Citation: WANG Ze-Lan, ZHOU Yan-Fen, MENG Zhe, LI Ji-Guang, LI He-Ping, REN Jian-Lin, LIU Wan-Yi. Determination of Trace Sulfonamides Antibiotics in Milk Using Polyaniline Silicon Magnetic Composite Selective Magnetic Solid Phase Extraction Combined with High Performance Liquid Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(1): 119-128. doi: 10.19756/j.issn.0253-3820.181478 shu

Determination of Trace Sulfonamides Antibiotics in Milk Using Polyaniline Silicon Magnetic Composite Selective Magnetic Solid Phase Extraction Combined with High Performance Liquid Chromatography-Mass Spectrometry

State Key Laboratory of High-Efficiency Utilization of Coal and Green Chemical Engineering, School of Chemistry and Chemical Engineering, Ningxia University, Yinchuan 750021, China

Received Date: 23 July 2018
Revised Date: 8 November 2018

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 21768003).

The multi-layer core-shell polyaniline silicon magnetic composites (Fe₃O₄@SiO₂@PANI) were prepared in situ by oxidation polymerization-coprecipitation of silicon magnetic particles with low temperature (0℃). The Fe₃O₄@SiO₂@PANI was used as the adsorbent for the selective magnetic solid-phase extraction (MSPE) of four trace sulfonamides (SAs) antibiotics in milk samples prior to high performance liquid chromatography with mass spectrometry (HPLC-MS). The synthesized nanocomposite sorbents were characterized by Fourier transform infrared spectra (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and vibrating sample magnetometry (VSM) techniques. The predominant variables affecting the extraction efficiency of the MSPE procedure were investigated and optimized via the response surface methodology. The optimal conditions for separation and preconcentration of trace sulfonamides in milk sample were as follows. About 15.0 mg of Fe₃O₄@SiO₂@PANI was dispersed into 10 mL of milk sample and shaken for 40 min. Then, the Fe₃O₄@SiO₂@PANI carrying sulfonamides was separated from the milk sample by an external magnetic field. Next, the sulfonamides were eluted from Fe₃O₄@SiO₂@PANI with 1.0 mL of methanol aqueous solution (7:3, V/V). Under the optimized conditions, an excellent linearity was observed in the range of 10-1500 μg/L for the four sulfonamides, with the correlation coefficients of 0.9976-0.9995. The limits of detections ranged from 1.3 μg/kg to 8.2 μg/kg. The mean recoveries at three spiked levels ranged from 69.7% to 99.6%. The relative standard deviations (RSDs) of intra-day and inter-day varied from 3.4%to 4.6%and 7.8% to 10.7%, respectively. The proposed method had low background and high selectivity and sensitivity, and was successfully applied to the simultaneous determination of four kinds of trace sulfonamides antibiotics in milk sample.
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