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Determination of twenty-two sulfonamide residues in pork by matrix solid phase dispersion-high pressure liquid chromatography-high resolution mass spectrometry spectrometry

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Journal: Shipin Anquan Zhiliang Jiance Xuebao
ISSN 2095-0381

Volume: 4;
Issue: 1;
Start page: 141;
Date: 2013;
Original page

Keywords: high resolution mass spectrometry | matrix solid phase dispersion | pork | sulfonamides

ABSTRACT
Objective To establish a method for determination of 22 sulfonamides in pork, including sulfabenzamide, sulfacetamide, sulfachloropyridazine, sulfadiazine, sulfadimethoxine, sulfamethazine, sulfamera-zinesulfadoxine, sulfamonomethoxine, sulfamethoxypyridazine, sulfamethoxydiazine, sulfamethoxazole, sulfamethizole, sulfamoxole, sulfaphenazole, sulfapyridine, sulfaquinoxaline, sulfathiazole, sulfisoxazole, sulfaguanidine, trimethoprim and sulfisomidine, with matrix solid phase dispersion and high pressure liquid chromatography-high resolution mass spectrometry. Methods Pork samples were mixed and grinded with solid-phase sorbent (Florisil), then put in a glass mortar. The mixture was packed as a solid phase extraction cartridge and eluted with 15 mL 1% acetic acid dichloromethane:ethyl acetate(1:3, v/v). The eluted materials were collected and evaporated to dry by nitrogen gas. The residues were dissolved in 1 mL acetonitrile: 10 mmol/L ammonium acetate (15:85, v/v) and 1mL n-hexane. After centrifugation, the lower solution was gone through a 0.22 μm filter membrane and then separated by Agilent Poroshell 120 EC-C18 column (2.1 mm×150 mm, 2.7 μm), after that it was determined by high resolution mass spectrometry. Results The linear range of 22 sulfonamides were 10~100 μg/kg, r>0.99. The recoveries of sulfamethizole, trimethoprim and sulfaguanidine were below 40%, the others were above 60%. The limits of quantitation were 5~10 μg/kg. Conclusion The advantages of this method are fast, efficient, less organic reagent and low cost. It is suitable for the determination of sulfonamides residues in pork.
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