摘要
本研究通过超声提取-固相萃取,建立了利用超高效液相色谱/串联质谱同时分析粪便、土壤和水体中25种兽药抗生素的方法,考察了串联SAX小柱对土壤样品和粪便样品的净化效果,以及正己烷提取对粪便样品提取液脱脂的净化效果。实验结果表明：本方法对25种兽药抗生素加标回收率为50.0%～121.9%,相对标准偏差为1.1%～14.7%（n=9）;土壤和粪便的方法检出限为0.0002～0.0560μg/kg,水体的方法检出限为0.002～0.28 ng/L;串联SAX强阴离子交换柱后,土壤样品的基质效应降低为75%～160%之间,粪便样品降低为55%～120%之间;粪便样品经正己烷脱脂后,基质效降为55%～120%之间。已将本方法应用于养殖场周边环境介质的检测。
A liquid chromatography-tandem mass spectrometric method was established for the determination of 25 kinds of veterinary antibiotics in manure,soil and water by ultrasonic-solid phase extraction. Purification efficiency of SAX cartridges for soil and manure samples extract and the procedure that manure samples defatted with hexane was also verified. The results showed that the average recoveries of the 25 target antibiotics were 50. 0%- 121. 9%,the relative standard deviations（ RSD） were 1. 1%- 14. 71%（ n = 9）,and the limits of detection（ LOD） ranged from 0. 0002- 0. 0560 μg / kg for soil and manure and ranged from0. 002- 0. 28 ng / L for water; After adding SAX cartridges,the matrix effects of manure samples reduced to 55%- 120%,and soil samples to 75%- 160%; after defatting by hexane extraction,the matrix effects of manure sample reduced to 55%- 120%. This method has been employed to detect the veterinary antibiotics in environmental samples of livestock farm.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2015年第1期13-20,共8页
Chinese Journal of Analytical Chemistry
基金
环保公益性行业科研专项(Nos.201109038
201309031)资助项目~~
关键词
抗生素
喹诺酮类
磺胺类
四环素类
大环内酯类
液相色谱-串联质谱
Antibiotics
Quinolones
Sulfonamides
Tetracyclines
Macrolides
Liquid chromatographytandem mass spectrometry
