【作者】 孙志文；

【导师】 肖希龙；

【作者基本信息】 中国农业大学 ， 基础兽医学， 2004， 硕士

【摘要】 异氯霉素（meta-nitrochloramphenicol,m-CAP）是气相色谱（GC）检测氯霉素残留的一种内标物，用它作内标物是氯霉素痕量分析中提高定量准确性的一种有效方法，本文成功合成了氯霉素的同分异构体—异氯霉素，用它来作为氯霉素的气相色谱定量与气相色谱／质谱（GC／MS）联用确证检测方法的内标物。 本文成功建立了鸡肌肉和肝脏组织中氯霉素的气相色谱定量与气相色谱／质谱联用确证检测方法。乙酸乙酯提取，正己烷脱脂后，乙酸乙酯液液分配，加入异氯霉素（m-CAP）标准溶液作为内标物，蒸干，Sylon BFT衍生化后加入甲苯、蒸馏水处理，吸取上层有机相，取3μl进GC分析，1μl进GC／MS分析。气相色谱微电子捕获检测器（μECD）定量，鸡肌肉在0.1μg·kg^-1、1μg·kg^-1、20μg·kg^-1三个添加水平，平均回收率范围在82.8％～94.4％之间，日内变异系数范围在2.0％～4.5％（n=5）之间，日间变异系数范围在2.1％～12.7％（n=3）之间，检测限0.04 μg·kg^-1。鸡肝脏在0.2μg·kg^-1、1μg·kg^-1、20μg·kg^-1三个添加水平，平均回收率范围在69.1％～83.5％之间，日内变异系数范围在3.2％～8.2％（n=5）之间，日间变异系数范围在2.7％～8.0％（n=3）之间，检测限0.12 μg·kg^-1。质谱定性，质谱系统选择负离子化学电离（NICIMS）模式，选择离子m／z468，466，360，358，322和304检测。并在0.1μg·kg^-1(肝脏0.2μg·kg^-1)、1μg·kg^-1、5μg·kg^-1三个添加水平对肌肉和肝脏成功进行了确证。 80只肉鸡分成3组，高剂量组(800 mg·kg^-1饲料)、低剂量组(200 mg·kg^-1饲料)和空白组，高、低剂量组连续饲喂添加氯霉素的饲料5天。试验结果表明，对照组中未检测出氯霉素残留。低剂量组，停药0h时，肌肉组织氯霉素平均残留水平为10.7μg·kg^-1；肝脏组织中氯霉素平均残留水平为0.73μg·kg^-1，停药12h时，肌肉中氯霉素平均残留水平为2.65μg·kg^-1，肝脏组织中未检出氯霉素残留，肌肉组织在停药8d时，未检测出氯霉素残留。高剂量组，停药0h时，肌肉组织氯霉素平均残留水平为42.1μg·kg^-1，肝脏组织中氯霉素平均残留水平为7.22μg·kg^-1，停药14d时，肌肉组织中未检测出氯霉素残留，而在停药24h时，肝脏组织已检测不到氯霉素残留。更多还原

【Abstract】 Meta-nitrochloramphenicol (m-CAP) is a kind of internal standards used in gas chromatography for chloramphenicol (CAP) residue detection. It is an effective method for increasing accuracy of quantitativeness in trace analysis by using m-CAP as an internal standard in Chloramphenicol residue analysis. m-CAP was prepared successfully in this study.In this paper a method was developed for determination of Chloramphenicol by gas chromatography and confirmation of Chloramphenicol by gas chromatography/mass spectrometry in broiler chicken muscles and livers.The tissues was extracted with ethyl acetate .The sample was defatted with hexane and extracted with ethyl acetate, then m-CAP was added to the sample, evaporated to dryness with nitrogen gas.Residue must be dry before adding Sylon N,O-Bis(trimethylsily) trifluoroacetamide (BFT).Added Sylon BFT.After derivatization, tolune and water were added directly to the sample .The organic layer was carefully removed.3ul analytes were determined by GC with micro electron capture detector(uECD) and 1ul confirmed by gas chromatography/ mass spectrometry. Analyzed by negative ion chemical ionization (NICIMS) with selected ion monitored.The ions with m/z 468,466,360,358,322,and 304 were monitor.The recoveries of analytes at the fortified level of 0.1ug. kg -1,1ug. kg-1,20 ug. kg-1 range from 82.8%~94.4% in the muscle , and at the fortified level of 0.2ug. kg-1, 1ug. kg-1,20 ug. kg-1 range from 69.1%-83.5% in the liver,respectively.Coefficents of variation for distribution,CVd,ranged from 2.0% to 4.5% in muscle, from 3.2% to 8.2% in liver,respectively.And for precision CVr,ranged from 2.1% to 12.7% in muscle,from 2.7% to 8.0% in liver,respectively.The limit of detection(LOD) is 0.04 ug. kg-1 in muscle, 0.12 u g. kg-1 in liver.In feeding trial,eighty chicken was divided into 3 groups,high dosage group(800 mg. kg-1 feed),low dosage group(200 mg. kg-1 feed) and blank group,medicated 5 days continually.After the drug withdrawal, the concentrations of the Chloramphenicol residue in muscle and in liver were detected by GC.Fortified low dosage group,the Chloramphenicol residues were 10. 7ug. kg-1 and 2. 65ug. kg-1 at 0,12 hours.at the 8 days,below the LOD in muscle, the Chloramphenicol residues were 0. 73ug. kg-1 at 0 hours, at 12 hours, below the LOD in liver.Fortified high dosage group.the Chloramphenicol residues were 42. lug. kg-1, at the 14 days,below the LOD in muscle. The Chloramphenicol residues were 7. 22ug. kg-1 at 0 hours, at 24 hours, below the LOD in liver.更多还原