分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
1期
13-20
,共8页
郭欣妍%王娜%郝利君%智勇%许静%王昝畅%单正军
郭訢妍%王娜%郝利君%智勇%許靜%王昝暢%單正軍
곽흔연%왕나%학리군%지용%허정%왕잠창%단정군
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
抗生素%喹諾酮類%磺胺類%四環素類%大環內酯類%液相色譜_串聯質譜
항생소%규낙동류%광알류%사배소류%대배내지류%액상색보_천련질보
Antibiotics%Quinolones%Sulfonamides%Tetracyclines%Macrolides%Liquid chromatography_tandem mass spectrometry
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。
本研究通過超聲提取_固相萃取,建立瞭利用超高效液相色譜/串聯質譜同時分析糞便、土壤和水體中25種獸藥抗生素的方法,攷察瞭串聯SAX小柱對土壤樣品和糞便樣品的淨化效果,以及正己烷提取對糞便樣品提取液脫脂的淨化效果。實驗結果錶明:本方法對25種獸藥抗生素加標迴收率為50.0%~121.9%,相對標準偏差為1.1%~14.7%(n=9);土壤和糞便的方法檢齣限為0.0002~0.0560μg/kg,水體的方法檢齣限為0.002~0.28 ng/L;串聯SAX彊陰離子交換柱後,土壤樣品的基質效應降低為75%~160%之間,糞便樣品降低為55%~120%之間;糞便樣品經正己烷脫脂後,基質效降為55%~120%之間。已將本方法應用于養殖場週邊環境介質的檢測。
본연구통과초성제취_고상췌취,건립료이용초고효액상색보/천련질보동시분석분편、토양화수체중25충수약항생소적방법,고찰료천련SAX소주대토양양품화분편양품적정화효과,이급정기완제취대분편양품제취액탈지적정화효과。실험결과표명:본방법대25충수약항생소가표회수솔위50.0%~121.9%,상대표준편차위1.1%~14.7%(n=9);토양화분편적방법검출한위0.0002~0.0560μg/kg,수체적방법검출한위0.002~0.28 ng/L;천련SAX강음리자교환주후,토양양품적기질효응강저위75%~160%지간,분편양품강저위55%~120%지간;분편양품경정기완탈지후,기질효강위55%~120%지간。이장본방법응용우양식장주변배경개질적검측。
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 from 0. 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.