中国农业科学 ›› 2007, Vol. 40 ›› Issue (4): 864-868 .

• 研究简报 • 上一篇    

猪可食组织中氯霉素和甲砜霉素残留检测气相色谱法建立

马素英,袁 霞,王玉莲,陶燕飞,陈冬梅,袁宗辉   

  1. 国家兽药残留基准实验室/农业部食品安全评价重点开放实验室/华中农业大学兽药研究所
  • 收稿日期:2005-05-11 修回日期:1900-01-01 出版日期:2007-04-10 发布日期:2007-04-10
  • 通讯作者: 袁宗辉

Development of a Gas Chromatography Method for the Determination of Chloramphenicol and Thiamphenicol Residues In Edible Tissues of Swine

  1. 国家兽药残留基准实验室/农业部食品安全评价重点开放实验室/华中农业大学兽药研究所
  • Received:2005-05-11 Revised:1900-01-01 Online:2007-04-10 Published:2007-04-10

摘要: 【目的】为检测猪可食用组织中氯霉素和甲砜霉素残留,建立了同时检测这两种残留药物的气相色谱方法。【方法】样品用乙酸乙酯提取、离心、蒸发、氯化钠溶液溶解,然后用预先活化的C18固相萃取小柱净化。用水淋洗、乙腈洗脱固相萃取柱。收集洗脱液,洗脱液吹干后和Sylon BFT(99+1)于70℃反应30 min。反应物用氮气吹干,重新溶解在正己烷和环己烷的混合溶液(6+4)中,终产物用气相色谱法分析。【结果】本法对猪肝脏和肌肉中氯霉素的检测限为0.5 μg•kg-1,定量限为1.0 μg•kg-1;对甲砜霉素的检测限为1.0 μg•kg-1,定量限为2.0 μg•kg-1。氯霉素在1.0~4.0 μg•kg-1和甲砜霉素在2.0~8.0 μg•kg-1添加浓度范围内,肝脏和肌肉组织中的回收率在70%~81%范围内,变异系数<16%。氯霉素和甲砜霉素标准溶液在10~640 μg•L-1浓度范围内线性关系良好(R2>0.998)。【结论】本方法简单、灵敏度高,适用于猪可食用组织中氯霉素和甲砜霉素的定量检测。

关键词: 氯霉素, 甲砜霉素, 残留, 猪, 可食组织, 气相色谱法

Abstract: Abstract:A Gas Chromatography method was developed to simultaneously determine chloramphenicol and thiamphenicol residues in edible tissues of swine, The residues were extracted with ethyl acetate and cleaned up by C18 solid phase extraction cartridge. Residues were reacted with BSTFA-TMCS(99:1)at 70℃ for 30min and then evaporated to dryness by nitrogen. The final solution were analysed by Gas Chromatography. The limits of detection of chloramphenicol in liver and muscle of swine are 0.5μg/kg and the limits of quantification are 1.0μg/kg, The limits of detection of thiamphenicol in liver and muscle of swine are 1.0μg/kg and the limits of quantification are 2.0μg/kg. The samples are fortified with chloramphenicol in the range of 1~4μg/kg and with thiamphenicol in the range of 2~8μg/kg, The recoveries are in the range of 70%~81% and the correlation coefficient are less than 16%. The calibration curves of chloramphenicol and thiamphenicol are linear (R2>0.998) in the range of 10μg/L~640μg/L. The method is simple and accurate enough to determine the residues of chloramphenicol and thiamphenicol in edible tissues of swine.

Key words: chloramphenicol, thiamphenicol, residues, edible tissues, swine, GC-ECD