分析测试学报2017，Vol.36Issue(2)：218-223,6.DOI:10.3969/j.issn.1004-4957.2017.02.011
QuEChERS结合柱净化的超高效液相色谱-串联质谱法测定有机肥中46种抗生素
Determination of 46 Antibiotics Residues in Organic Fertilizer by UPLC-MS/MS with QuEChERS Combined with Column Purification
摘要
Abstract
A confirmative method was developed for the simultaneous determination of 46 antibiotics,including sulfonamides,quinolones and macrolides in organic fertilizer by ultrahigh performance liquid chromatography-tandem massspectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile-EDTA buffer solution (pH 10.0),and separated by centrifugation after salting-out.The upper acetonitrile layer was purified by the QuEChERS steps with sorbents.The buffer solution layer was purified with solid-phase extraction cartridge.The separation of target drugs was performed on an ACQUITY UPLC BEH C1scolumn using a mobile phase consisting of 2 mmol/L ammonium acetate with 0.1％ formic acid and methanol by gradient elution.The analysis of target compounds was carried out with positive electrospray ionization (ESI +)source under multiple reaction monitoring (MRM) mode.The matrix-matched external standard calibration was used for quantification.Good linearities for the 46 antibiotics were achieved over the concentration of 1-200 μg/L,with correlation coefficients (r2) of 0.996 6-0.999 9.The recoveries of sulfonamides,quinolones and macrolides at spiked levels of 25,100,400 μg/kg were in the range of 67.8％-95.6％,65.6％-89.4％ and 66.6％-107.8％,respectively,with relative standard deviations(RSDs) of 0.4％-11.9％.The limits of detection (LOD,S/N =3) were 0.6-4.6 μg/kg,and the limits of quantitation(LOQ,S/N=10) were 2.1-15.4 μg/kg.关键词
超高效液相色谱-串联质谱法(UPLC-MS/MS)/抗生素残留/有机肥/QuEChERS结合柱净化Key words
ultrahigh performance liquid chromatography-tandem massspectrometry(UPLC-MS/MS)/antibiotics residues/organic fertilizer/QuEChERS combined with column purification分类
化学化工引用本文复制引用
汪建妹,刘艳平,陈静,吴慧珍,夏魏,李祖光,钱鸣蓉..QuEChERS结合柱净化的超高效液相色谱-串联质谱法测定有机肥中46种抗生素[J].分析测试学报,2017,36(2):218-223,6.基金项目
农业部公益性行业专项(201303091) （201303091）
浙江省自然科学基金(LY14B070008) （LY14B070008）
省部共建国家重点实验室培育基地项目(2010DS700124-ZZ1602) （2010DS700124-ZZ1602）
浙江省农业科学院中美三方合作项目(2010DS700124-ZM1604) （2010DS700124-ZM1604）
宁波科技项目(2013C11024) （2013C11024）
