Rapidly Simultaneous Determination of 27 Antibiotic Residues in Milk Using Microwave Assisted Hollow Fiber Liquid Phase Microextraction Coupled With Liquid Chromatography Tandem Mass Spectrometry
A novel sample preparation technique based on microwave assisted extraction coupled with hollow fiber liquid phase microextraction(HF-LPME) was studied.Octanol/toluene(1∶1,V/V) was poured into a hollow fiber as accepted phase,and both ends were sealed.The fiber was immerged into donated phase for extraction.Twenty-seven target compounds were simultaneously extracted during 12.67 min under the conditions of continuous 700 r/min stirring and intermittent microwave(MW) irradiation.The method based on MW assisted HF-LPME coupled with LC-MS/MS detection was developed.It was successfully applied to simultaneous analysis of 27 antibiotics(9 quinolones,15 sulfanilamides and 3 macrolides) residues in milk.The matrix-matched calibrations were respectively used to quantify these compounds,and the linear range was 0.2-5.0 μg/kgwith the correlation coefficients above 0.99(r≥0.99,n=3).The quantitative limit(LOQ,S/N=10) was 0.036-0.568 μg/kg.Method validation was carried out at three standard addition levels of 0.5,1.0,2.0 μg/kgand the recovery was 49.0%-115.0% with relative standard deviations(RSDs) of 0.9%-21.1%.