固相萃取-气相色谱-质谱联机分析蜂蜜中的氯霉素残留量  

DETERMINATION OF CHLORAMPHENICOL RESIDUE IN HONEY BY COUPLING SOLID-PHASE EXTRACTION WITH GAS CHROMATOGRAPHY-MASS SPECTROMETRY

作　　者：刘宜孜[1] 谢孟峡[1] 韩杰[1] 刘媛[1] 邱月明[1] 丁雅韵[1] 张雷[1] 

机构地区：[1]北京师范大学分析测试中心,北京100875

出　　处：《北京师范大学学报（自然科学版）》2004年第2期232-236,共5页Journal of Beijing Normal University(Natural Science)

基　　金：国家科技攻关计划资助项目 ( 2 0 0 1BA80 4A18)

摘　　要：利用固相萃取气相色谱质谱联机分析蜂蜜中的氯霉素残留量 .对氯霉素在固相萃取柱上的保留行为进行了研究 ,优化固相萃取条件 ,发现不同浓度的氯霉素在硅胶柱和C18柱上的回收率均在 90 %以上 ,蜂蜜加标的回收率为 80 %～ 95 % ,相对标准偏差为 7.2 %～ 18.2 % ,最低检出限为 0 .1μg·kg- 1.对氯霉素的三甲基硅烷化衍生物采用选择离子的模式进行检测 (m/Z =4 6 6 ,4 6 8,4 70 ) ,衍生物的峰面积与样品质量浓度在 0 .5 5～ 2 2 0 μg·L- 1范围内呈良好的线性关系 ,线性回归系数为 0 .9998.Solid phase extraction (SPE) and gas chromatography mass spectrometric method are applied for the determination of residues of chloramphenicol in honey samples. The retention behavior of chloramphenicol on SPE columns is investigated. It is found that the recovery of different quantities of chloramphenicol on the SI 1 columns is above 90%. The average recovery of chloramphenicol in honey samples is 73% 95%. The relative standard deviation is 7.2% 18.2% and the detection limit is 0.1 μg·kg -1 for honey samples. The selected ion mode (SIM) detection method (ions selected: 466,468,470) is used for the detection of the chloramphenicol derivatives. There is a good linear correlation ( r= 0.999 8) between the peak areas and the concentration of chloramphenicol in the range of 0 55 220 μg·L -1 .

关 键 词：氯霉素 气相色谱-质谱联机 固相萃取 蜂蜜 

分 类 号：O657.63[理学—分析化学] O658.2[理学—化学]