龚兰, 栾枫婷, 温天锐, 陈明, 邓博文, 张泽璟, 魏瑞成, 王冉. Analysis of Macrolide Antibiotics in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry Based on Solid Phase Extraction[J]. 2020, 39(7): 874-880.
龚兰, 栾枫婷, 温天锐, 陈明, 邓博文, 张泽璟, 魏瑞成, 王冉. Analysis of Macrolide Antibiotics in Feeds by High Performance Liquid Chromatography-Tandem Mass Spectrometry Based on Solid Phase Extraction[J]. 2020, 39(7): 874-880.DOI: doi:10.3969/j.issn.1004-4957.2020.07.008.
建立了添加剂预混合饲料、精料补充饲料、配合饲料和浓缩饲料中7种大环内酯类药物(替米考星、罗红霉素、螺旋霉素、泰乐菌素、红霉素、克拉霉素和阿奇霉素)含量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。饲料样品经1%氨化乙腈提取,Oasis PRiME HLB固相萃取柱净化后,采用ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the simultaneous determination of seven macrolide antibiotics
ie.tilmicosin
roxithromycin
spiramycin
tylosin
erythromycin
clarithromycin and azithromycin in additive premix
concentrate supplement
complete feed and concentrated feed.The samples were extracted with 1% ammoniated acetonitrile solution
followed by Oasis PRiME HLB solid phase extraction for further purification.The analytes were separated on an ACQUITY UPLC BEH C18 column(2.1 mm×100 mm
1.7 μm) by gradient elution using 0.1% formic acid solution and acetonitrile as mobile phases
then analyzd by MS/MS with electrospray ionization in positive mode
and quantified by external standard method.Results showed that there were good linear relationships for 3 target analytes
ie.tilmicosin
spiramycin and erythromycin in the concentration range of 0.5-50 μg/L(r2>0.99) and for the other 4 target analytes in the range of 0.25-50 μg/L(r2>0.99).The limits of detection and the limits of quantitation were in the ranges of 1.25-2.5 μg/kg and 2.5-5.0 μg/kg
respectively.At three spiked levels of 5
10 and 50 μg/kg
the average recoveries for target compounds ranged from 61.4% to 103% with relative standard deviations of 0.43%-15%.The developed method is simple
rapid
sensitive and low matrix interference
and it is suitable for the routine supervision and quantitative detection of macrolide antibiotics in different feeds.