气相色谱-质谱联用法测定动物组织中氯霉素、氟甲砜霉素和甲砜霉素的残留量  

Simultaneous Determination of Chloramphenicol,Thiamphenicol,and Florfenicol Residues in Animal Tissues by Gas Chromatography/Mass Spectrometry

作　　者：李鹏[1] 邱月明[1] 蔡慧霞[1] 孔莹[1] 唐英章[1] 王大宁[1] 谢孟峡[2] 

机构地区：[1]中国检验检疫科学研究院,北京100025 [2]北京师范大学分析测试中心,北京100875

出　　处：《色谱》2006年第1期14-18,共5页Chinese Journal of Chromatography

基　　金：科技部食品安全研究专项课题"兽药残留检测技术研究"和质检总局重点课题(2001BA804A18)

摘　　要：建立了气相色谱-负离子化学电离源质谱同时测定动物组织中氯霉素（CAP）、甲砜霉素（TAP）和氟甲砜霉素（FF）残留量的方法。样品用乙酸乙酯提取，正己烷分配去脂肪。再用Florisil柱进一步净化。甲苯作为反应介质，用N，O-双（三甲基硅基）三氟乙酰胺（BSTFA）-三甲基氯硅烷（TMCS）（体积比为99：1）进行硅烷化处理，用间硝基氯霉素（m—CAP）作为内标进行测定。CAP的检测限可达到0．03μg／kg，TAP和FF的检测限可达到0．2μg／kg；上述3种药物的标准曲线的线性相关系数均大于0．99。CAP，FF和TAP的批内测定的精密度（以相对标准偏差表示）依次为5．5％，10．4％和8．8％；批间测定的精密度依次为7．4％，20．7％和19．1％。回收率为80．0％-111．5％。相对标准偏差为1．2％-15．4％。该方法前处理步骤简单，处理后杂质干扰少。灵敏度高。适用性强。可用于猪肉及禽类、水产品等多种动物组织中氯霉素类药物残留的检测。A method was developed for the simultaneous determination of chloramphenicol （CAP）, thiamphenicol （TAP）, and florfenicol （FF） residues in animal tissues using gas chromatography/mass spectrometry （GC/MS） with chemical ionization source in negative mode. The homogenized samples were extracted with ethyl acetate and the extracts were partitioned with n-hexane to remove lipids. Further cleanup was performed on a florisil cartridge and the purified samples were derivatized with Sylon BFT [ N, O-bis （trimethylsilyl） trifiuoroacetamide （BSTFA）-trimethylchlorosilane （TMCS）, 99： 1, v/v ] in toluene. Meta-nitrochloramphenicol （m-CAP） was used as the internal standard for the determination. Selected ion monitoring （SIM） was used for detection, ions were chosen, respectively, for the monitoring at m/z 432, 466,468,470 for m-CAP, m/z 376, 378, 466, 468 for CAP, m/z 409, 411, 499, 501 for TAP, and m/z 339, 341,429,431 for FF. Quantitative ions were selected at m/z 466 for CAP and m- CAP, at m/z 339 for FF and at m/z 409 for TAP. The detection limits were 0.03 μg/kg for CAP, 0.2 μg/kg for FF and TAP. The correlation coefficients were above 0.99 for the calibration curves of the medicines. The linear ranges were 0.1 - 8.0 μg/kg for CAP and 0.2 - 4.0 μg/kg for FF and TAP. The reproducibilities of the compounds within a batch were 5.5%, 10. 4%, and 8.8% for CAP, FF, and TAP respectively, while the corresponding values between the batches were 7.4%, 20.7%, and 19. 1%. The recoveries were 80. 0% - 111.5%, and the relative standard deviations were 1.2% - 15.4%. The method is applicable for detection of the residues in animal derived food, such as pork, poultry and aquatic products.

关 键 词：气相色谱-质谱 氯霉素 氟甲砜霉素 甲砜霉素 固相萃取 

分 类 号：O658[理学—分析化学]