摘要
Abstract
The use of salting-out assisted liquid-liquid extraction ( SALLE) combined with UPLC-MS/MS has been evaluated for the determination of tetrac≥clines in milk powder. The samples were extracted with Na2 EDTA-Mcllvaine buffer, and then the target anal≥tes were extracted with acetonitrile assisted with ( NH4 )2 SO4 . After concentrated, the target anal≥tes were separated on a BEH C18 column with gradient elution using acetonitrile and water containing volume fraction 0. 1% formic acid as mobile phase. MS detection was performed with the positive ion mode in multi-reaction monitoring. The samples were quan-tified with external standard method. The result showed that, under the assisted with ( NH4 )2 SO4 , the extraction and purification effect of acetonitrile was improved. The limit of detection was 0. 36 μg/kg, which was much lower than 50 μg/kg for the solid-phase extraction method. The linear range was from 1 to 100 μg /kg with the correlation coefficient R>0. 999. The recoveries of the method were ranged from 71. 88% to 107. 13% at the spiked levels of 1, 5, 50 μg/kg and the relative standard deviation was less than 8% . This method was simple, sensitive, economical, reliable and environmentall≥ friendl≥. The method was suitable for the qualitative and quantitative of tetrac≥clines in milk powder.关键词
盐析/液液萃取/超高效液相色谱-串联质谱法/四环素类抗生素/婴儿配方奶粉Key words
salting-out/liquid-liquid extraction/UPLC-MS/MS/tetrac≥clines/infant formula分类
轻工纺织
