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Study On GC/MS For Chloramphenicol In Feed

Posted on:2009-09-23Degree:MasterType:Thesis
Country:ChinaCandidate:H Y LiuFull Text:PDF
GTID:2143360302958132Subject:Farming
Abstract/Summary:PDF Full Text Request
Chloramphenicol(CAP) was a broad-spectrum antibiotic which used to feed.It plays an important role of treatment and prevention about animal infectious disease.However,it was easy accumulated in animal and human body,which could lead to agranulocytosis, aplastic anemia and the serious toxicity of digestive system.In recent years,the countries and international organizations were very concerned about CAP residues in food in the world,and to establish a strict standard limit.European Union,United States,China and other countries hold the CAP as banned drugs.With the critical situation of food security, therefore,it was significant to detect the content of CAP in feed.Gas chromatagraphy -mass spectrometry(GC/MS) and Solid phase extraction method for determining CAP in feed were ensured.The results as follow:1 Establishment of GC/MS method for determining CAPGas chromatogram condition:the chromatographic was HP-5MS5% benz-Methylpolysiloxane,and the inner diameter and thickness were 30m×0.25mm and 0.25μm.The temperature of sample introduction was 250℃and temperature gradient were 100℃(1min) 30℃280℃(9min).The flow rate was 0.8mL/min and the volume of sample introduction was 1.0μL.Mass spectrometry condition:the sample ion source was chemi-ionization.The source temperature and transmission temperature were 150℃and 250℃.The detect voltage was 500V.Selecting a mode of ion collection,the selective e/m were 73,147,221,281,365 and 429.The detection limit of this method was down to 0.1ng/g.The calibration curve was linear in the range of 0.5~200ng/g.The recoveries were 78.2~89.3%,The relative standard deviation(n=5) was 4.34~6.03%.At the0.5,5,10ng/g additional concentration,the coefficient of variability within day was 5.67%,4.50%,and 4.35%,the coefficient of variability between day and day was 5.04%,4.19%,and 3.97%.2 Establishment of sample pretreatment technique in feedSample extraction:Acetate ester and phosphate buffer were used to extract the CAP of feed.Solid phase extraction:The extracts further were purified and enriched by silica and C18 solid phase extraction cartridges.The final extracts were derivatization with BSTFA and CAP was analyzed by GC/MS.The results showed that a new method which to detect CAP of feed was established in this study.This way will provide a new method for determination of CAP in feed.The method had advantage of sensitive,practicable,simple and so on.This way could detect CAP in variety of feed.The establishment of the method had a significance for food security and people healthy.
Keywords/Search Tags:CAP, GC/MS, Solid phase extraction, detect
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