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高效液相色谱同时检测鱼肉组织中4种磺胺与甲氧苄啶的残留量
引用本文:朱晓华,翁棋兰,王静,刘畅,吴光红.高效液相色谱同时检测鱼肉组织中4种磺胺与甲氧苄啶的残留量[J].南京农业大学学报,2009,32(4).
作者姓名:朱晓华  翁棋兰  王静  刘畅  吴光红
作者单位:1. 江苏省水产质量检测中心,江苏 南京 210017;农业部渔业产品质量监督检验测试中心,南京,江苏 南京 210017
2. 南京福润德动物药业有限公司,江苏 南京,210007
基金项目:江苏省科技公共服务平台项目 
摘    要:建立了同时测定鱼肉组织中4种磺胺(磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲恶唑)和甲氧苄啶残留量的高效液相色谱法.鱼肉组织用乙腈提取后经乙腈饱和的正己烷去脂,过HLB柱净化,甲醇洗脱,减压浓缩蒸干,流动相(乙腈+1%乙酸,体积比为10∶90)定容,用带DAD检测器的高效液相色谱仪在272 nm波长下检测,流动相采用梯度洗脱.结果显示:4种磺胺和甲氧苄啶分别在0025~10 μg·mL-1和005~20 μg·mL-1范围内呈良好线性关系,相关系数(r)为0999;4种磺胺和甲氧苄啶分别在002、010和020 mg·kg-1和004、020和040mg·kg-1 3个浓度水平下的添加回收率为752%~979%,变异系数为28%~100%(n=6);根据3倍信噪比计算,磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲基嘧啶、磺胺甲恶唑和甲氧苄啶的最低检测限分别为0006、0007、0008、0008和0019mg·kg-1.

关 键 词:磺胺嘧啶  磺胺甲基嘧啶  磺胺二甲基嘧啶  磺胺甲恶唑  甲氧苄啶  罗非鱼  残留  高效液相色谱法

Simultaneous determination of 4 sulfonamides and trimethoprim residues in fish tissues by HPLC
ZHU Xiao-hua,WENG Qi-lan,WANG Jing,LIU Chang,WU Guang-hong.Simultaneous determination of 4 sulfonamides and trimethoprim residues in fish tissues by HPLC[J].Journal of Nanjing Agricultural University,2009,32(4).
Authors:ZHU Xiao-hua  WENG Qi-lan  WANG Jing  LIU Chang  WU Guang-hong
Abstract:The simultaneous determination of sulfonamides and trimethoprim residues in freshwater fishes by HPLC was established. Drugs in samples were extracted with acetonitrile and defatted by acetonitrile-saturated n-hexane, and then the suptants was cleaned up with a HLB column and eluted with methanol and evaporated. The residues was dissolved in the mobile phase. The results indicated that the working curves were linear (r=0. 999) in the range of 0. 025 -1. 0 μg· mL~(-1) for the 4 sulfonamides and 0. 05 -2. 0 μg · mL~(-1) for trimethoprim. When spiked with 0. 02, 0. 10, 0. 20 mg · kg~(-1) of 4 sulfonamides and 0. 04, 0. 20, 0. 40 mg · kg~(-1) of trimethoprim, the average recoveries of samples ranged from 75. 2% to 97. 9% and the RSD (n = 6) were 2. 8%-10. 0% . The limit of detection ( LOD) as estimated by 3 times signal to noise method for sulfadiazine, sulfamerazine, sulfadimidine, sulfame-thoxazole, trimethoprim was 0. 006, 0.007, 0.008, 0. 008 and 0. 019 mg ·kg~(-1), respectively.
Keywords:sulfadiazine  sulfamerazine  sulfadimidine  sulfamethoxazole  trimethoprim  tilapia  residue  HPLC
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