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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
引用本文:李鹏,邱月明,蔡慧霞,孔莹,唐英章,王大宁,谢孟峡.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[J].色谱,2006,24(1):14-18.
作者姓名:李鹏  邱月明  蔡慧霞  孔莹  唐英章  王大宁  谢孟峡
作者单位:1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2.Analytical & Testing Center of Beijing Normal University, Beijing 100875, China
基金项目:科技部专项基金;质检总局资助项目
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0.03 μg/kg,TAP和FF的检测限可达到0.2 μg/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。

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  
文章编号:1000-8713(2006)01-0014-05
收稿时间:2005-02-21
修稿时间:2005年2月21日

Simultaneous Determination of Chloramphenicol, Thiam-phenicol, and Florfenicol Residues in Animal Tissues by Gas Chromatography/Mass Spectrometry
LI Peng,QIU Yueming,CAI Huixia,KONG Ying,TANG Yingzhang,WANG Daning,XIE Mengxia.Simultaneous Determination of Chloramphenicol, Thiam-phenicol, and Florfenicol Residues in Animal Tissues by Gas Chromatography/Mass Spectrometry[J].Chinese Journal of Chromatography,2006,24(1):14-18.
Authors:LI Peng  QIU Yueming  CAI Huixia  KONG Ying  TANG Yingzhang  WANG Daning  XIE Mengxia
Institution:1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2.Analytical & Testing Center of Beijing Normal University, Beijing 100875, China
Abstract: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) trifluoroacetamide (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 microg/kg for CAP, 0.2 microg/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 microg/kg for CAP and 0.2 - 4.0 microg/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.
Keywords:gas chromatography/mass spectrometry(GC/MS)  chloramphenicol  florfenicol  thiamphenicol  solid-phase extraction
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