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

作  者: ; ; ; ; ; ;

机构地区: 华中农业大学动物医学院国家兽药残留基准实验室

出  处: 《中国农业科学》 2007年第4期864-868,共5页

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SylonBFT(99+1)于70℃反应30min。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0.5μg·kg-1,定量限为1.0μg·kg-1;对甲砜霉素的检测限为1.0μg·kg-1,定量限为2.0μg·kg-1。氯霉素在1.0~4.0μg·kg-1和甲砜霉素在2.0~8.0μg·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10~640μg·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。 [Objective] A Gas Chromatography method was developed to simultaneously determine chloramphenicol and thiamphenicol residues in edible tissues of swine. [ Method ]The samples were extracted using ethyl acetate, centrifuged, evaporated, reconstituted in sodium chloride solution and then passed through preconditioned C18 solid phase extraction (SPE) cartridge. The SPE column was washed with water and eluted with acetonitrile. The elutant was collected, evaporated, and reacted with Sylon BFT at 70℃ for 30min. The derivative was evaporated dry, redissolved in hexane-cyclohexane (6+4) and centrifuged. The final solution was analyzed by Gas Chromatography. [Result] The limits of detection of chloramphenicol in liver and muscle of swine was 0.5 μg·kg^-1 and the limits of quantification was 1.0 μg·kg^-1, The limits of detection of thiamphenicol in liver and muscle of swine was 1.0 μg·kg^-1 and the limits of quantification was 2.0 μg·kg^-1. The samples were spiked with chloramphenicol in the range of 1-4 μg·kg^-1 and with thiamphenicol in the range of 2-8 μg·kg^-1. The recovery rate was in the range of 70%-81% and the correlation coefficient was less than 16%. The calibration curves of chloramphenicol and thiamphenicol were linear (R2〉0.998) in the range of 10-640 μg·kg^-1 [Conclusion]The method was simple and accurate enough to determine the residues of chloramphenicol and thiamphenicol in edible tissues of swine.

关 键 词: 氯霉素 甲砜霉素 残留 可食组织 气相色谱法

领  域: [农业科学] [农业科学] [农业科学]

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