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高效液相色谱法测定动物组织中3-甲基喹喔啉-2-羧酸残留量
Determination of the Marker Residue of Olaquindox,Methyl-3-quinoxaline-2-carboxylic Acid in Animal Edible Tissues Using High Performance Liquid Chromatography

作  者: ; ; ; (吴玉杰); (刘军义);

机构地区: 广西出入境检验检疫局广西南宁530021

出  处: 《分析科学学报》 2009年第4期427-430,共4页

摘  要: 本文建立了猪、鸡、鱼肌肉及猪、鸡肝脏组织中喹乙醇代谢残留标识物3-甲基喹喔啉-2-羧酸残留量的高效液相色谱分析方法。样品在酸性环境水解,经乙酸乙酯、磷酸盐缓冲溶液依次提取,Oasis MAX固相萃取柱净化,高效液相色谱紫外测定(HPLC-UV)。3-甲基喹喔啉-2-羧酸标准曲线相关系数(r^2)为0.9992(10~1000μg/L);不同动物组织样品中3-甲基喹喔啉-2-羧酸工作曲线相关系数(r)为0.9995~0.9997(2-100μg/kg)。在2~100μg/kg浓度范围,3-甲基喹喔啉-2-羧酸回收率为69%~104%,日内相对标准偏差〈15%,日间相对标准偏差〈20%。检出限(CCα)为1.2~4.3μg/kg,定量限(CCβ)为2.0~5.6μg/kg。 A method was developed for the quantitative determination of methyl-3-quinoxaline-2-carboxylic acid (MQCA), the metabolite that has been designated as the marker residue for olaquindox in swine tissue. This is the first report on simultaneous determination of MQCA in pork, chicken, fish and porcine, chicken livers. Samples were deproteinated with 5% metaphosphoric acid in 10% methanol followed by liquid-liquid extraction. Further clean-up was performed by solid phase extraction (SPE) through mixed mode anion-exchange columns (Oasis MAX SPE). Analysis was performed with RP-C18 column HPLC coupled to UV detector. The method has good linearity ranged from 2 to 100 μg/kg in tissues with recoveries from 69% to 104%, inter-day RSDs less than 15% and intra-day RSDs less than 20%, and the detection limit (CCα) (1.2-4.3 μg/kg) and the quantitation limit (CC/β) (2.0-5.6 μg/ kg) have been obtained in different tissues.

关 键 词: 喹乙醇 甲基喹喔啉 羧酸 固相萃取 高效液相色谱法 动物组织

领  域: [理学] [理学]

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