猪食用组织中喹喔啉-2-羧酸的高效液相色谱检测方法  

Liquid Chromatographic Determination of Quinoxaline-2-Carboxylic Acid in Edible Swine Tissues

作　　者：邱银生[1] 袁宗辉[1] 殷居易[1] 

机构地区：[1]华中农业大学兽药研究所,湖北武汉430070

出　　处：《兽医大学学报》2003年第3期286-288,共3页

基　　金：农业部兽药残留检测方法标准资助项目 ( 2 0 0 1年 )

摘　　要：为了监测猪食用组织中卡巴氧 (carbadox)的残留 ,建立了检测猪肝脏、肾脏、肌肉等组织中卡巴氧的标示残留物喹喔啉 - 2 -羧酸 (Quinoxaline- 2 - carboxylic acid,QCA)的高效液相色谱法。组织样品经碱水解 ,液 -液分配提取 ,用离子交换色谱柱净化 ,洗脱液作浓缩后用甲醇溶解进行测定。色谱柱为 ODS C1 8柱 ;流动相为甲醇 -水 (体积比 4 0∶ 6 0 ) ,每 1L中加入 8m L冰乙酸 ,流速为 1 .0 m L / min;定量分析用紫外检测器 ,波长 32 0 nm,确证性分析用二极管阵列检测器 ,波长 2 5 0～ 5 0 0 nm。喹喔啉 - 2 -羧酸工作液质量浓度在 0 .0 3～ 0 .96 mg/ L 范围内 ,药物峰面积与浓度呈良好的线性关系 ,相关系数 r=0 .9999。组织中添加药物的质量分数为 0 .0 1 5、0 .0 3、0 .0 6μg/ g时 ,肝脏样品回收率分别为 (73.5 5±9.4 6 ) %、(80 .33± 1 4 .95 ) %、(75 .84± 7.4 2 ) % ;肾脏样品分别为 (70 .89± 1 0 .33) %、(74 .89± 7.1 9) %、(83.33±1 0 .6 8) % ;肌肉样品分别为 (6 9.4 9± 7.2 6 ) %、(6 6 .4 4± 5 .0 9) %、(6 2 .1 1± 6 .0 8) %。本方法条件下 ,3种组织中药物最低检出质量分数均为 0 .0 1 5 μg/ g,回收率测定的日内及日间相对偏差 (RSD)分别 <1 8%和 <2 0 %。当组织中药物质量分数达A HPLC method for determination of quinoxaline 2 carboxylic acid (QCA) in swine liver,kidney,and muscle had been developed.Tissue samples were subjected to alkaline hydrolysis,liquid liquid extraction,ion exchange chromatography and further extraction to concentrate the analyte.Chromatographic column was packed with ODS C 18 .Mobile phase was a mixture of methanol water(40/60,V/V)with 0 8% acetic acid,and pumped at 1 0 mL per min.Its residue level was determined by HPLC with UV detection.Suspect positive peaks were identified with diode array detection.The response for QCA was linear in the range of 0 03～0 96 μg/mL,with a correlation coefficient>0 999.Validation exercises were carried out on batches of recovery samples,relative standard deviation for within day and between day were below 18% and 20%,respectively.Recoveries of QCA spiked to tissue were respectively 73 55±9 46%、80 33±14 95% and 75 84±7 42% for liver samples,70 89±10 33、74 89±7 19% and 83 33±10 68% for kidney samples,69 49±7 26%、66 44±5 09% and 62 11±6 08% for muscle samples when fortified with 0 015、0 03、0 06 μg/g,The minimum detection limit of QCA residues in tissues was at the level of 0 015 μg/g.

关 键 词：猪 食用组织 喹喔啉-2-羧酸 高效液相色谱检测方法 卡巴氧 饲料添加剂 残留 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] S854.4[轻工技术与工程—食品科学与工程]