色谱

色谱

• 研究论文 • 上一篇    下一篇

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

李鹏1,2,邱月明1,蔡慧霞1,孔莹1,唐英章1,王大宁1,谢孟峡2

  

  1. 1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2.Analytical & Testing Center of Beijing Normal University, Beijing 100875, China
  • 收稿日期:2005-02-21 修回日期:2005-11-18 出版日期:2006-01-30 发布日期:1987-09-25
  • 通讯作者: 李鹏

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

LI Peng1,2, QIU Yueming1, CAI Huixia1, KONG Ying1, TANG Yingzhang1, WANG Daning1, XIE Mengxia2   

  1. 1.Chinese Academy of Inspection and Quarantine, Beijing 100025, China; 2.Analytical & Testing Center of Beijing Normal University, Beijing 100875, China
  • Received:2005-02-21 Revised:2005-11-18 Online:2006-01-30 Published:1987-09-25

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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: 氟甲砜霉素, 固相萃取
, 甲砜霉素, 氯霉素, 气相色谱-质谱

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 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.

Key words: chloramphenicol, florfenicol, solid-phase extraction , thiamphenicol, gas chromatography/mass spectrometry(GC/MS)