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建立了养殖水体及沉积物中11种磺胺化合物的高效液相色谱?柱后衍生分析方法。养殖水体过滤后采用HLB固相萃取柱进行净化、富集;沉积物采用甲醇/EDTA?Mcllvaine缓冲液(1∶1, v/v)提取,HLB固相萃取柱净化富集。经高效液相色谱分离,用荧光胺衍生试剂进行柱后衍生,荧光检测器检测。对柱后衍生系统参数进行了优化,确定了荧光胺溶液的浓度、流速和反应温度分别为0?2 g/L、0?15 mL/min和50℃,磺胺化合物在0?01~1?0 mg/L范围内线性显著,其相关系数r2值大于0?99995。11种磺胺类药物在养殖水体和沉积物中的加标回收率分别为79?3%~100?7%和74?6%~95?3%,相对标准偏差为2?2%~11?0%和2?6%~10?3%,检出限( LOD, S/N=3)为0?9~5?5 ng/L和0?3~1?3μg/kg,定量限( LOQ, S/N=10)为3?0~18?1 ng/L和1?0~4?4μg/kg。该法可应用于养殖环境中磺胺类药物的定性定量检测,具有较好的实用性。

An analytical method was developed for the determination of 11 sulfonamide com?pounds in aquaculture water and sediments by high performance liquid chromatography ( HPLC) coupled with post?column derivatization. The filtered water sample was purified and concentrated with HLB cartridge, while the sediment sample was extracted with a mixture of methanol and EDTA?Mcllvaine buffer (1∶1, v/v), and then purified and enriched through HLB solid?phase extraction. The sulfonamides were separated on a C18 column by HPLC and on?line derivatized with a fluorescamine and detected with a fluorescence detector. The parameters of post?column derivatization system were optimized, and the fluorescamine solution concentra?tion, velocity of reagent solution and reaction temperature were 0?2 g/L, 0?15 mL/min and 50℃, respectively. The calibration curves of the method showed good linearity in the range of 0?01-1?0 mg/L, with the correlation coefficients ( r2 ) all above 0?999 95. The recoveries were 79?3%-100?7% and 74?6%-95?3% with RSD values of 2?2%-11?0% and 2?6%-10?3% for the 11 sulfonamides in aquaculture water and sediments, respectively. The respective limits of detec?tion ( LODs, S/N=3) were 0?9-5?5 ng/L and 0?3-1?3 μg/kg and the limits of quantification ( LOQs, S/N=10) were 3?0-18?1 ng/L and 1?0-4?4 μg/kg. The method can be applied to the determination of sulfonamides in the aquaculture environment, and it has a good practicability.

参考文献

[1] Rodgers C;Furones M D.[J].Opt Medit,2009A/86:41.
[2] Holmstrom K;Graslund S;Wahlstrom A;Poungshompoo S;Bengtsson BE.Antibiotic use in shrimp farming and implications for environmental impacts and human health[J].International Journal of Food Science and Technology,20033(3):255-266.
[3] Tamtam F;Mercier F;Le Bot B;Eurin J;Dinh QT;Clement M;Chevreuil M.Occurrence and fate of antibiotics in the Seine River in various hydrological conditions[J].Science of the Total Environment,20081(1):84-95.
[4] Chang H;Hu J Y;Wang L Z.[J].Chinese Science Bulletin,200853(04):514.
[5] Schwaiger J;Ferling H;Mallow U;Wintermayr H;Negele RD.Toxic effects of the non-steroidal anti-inflammatory drug diclofenac Part 1: histopathological alterations and bioaccumulation in rainbow trout[J].Aquatic Toxicology,20042(2):141-150.
[6] Mimeault C;Woodhouse AJ;Miao XS;Metcalfe CD;Moon TW;Trudeau VL.The human lipid regulator, gemfibrozil bioconcentrates and reduces testosterone in the goldfish, Carassius auratus[J].Aquatic Toxicology,20051(1):44-54.
[7] 何秀婷;王奇;聂湘平;杨永涛;程章.广东典型海水养殖区沉积物及鱼体中磺胺类药物的残留及其对人体的健康风险评价[J].环境科学,2014(7):2728-2735.
[8] 阮悦斐;陈继淼;郭昌胜;陈珊珊;王少特;王玉秋.天津近郊地区淡水养殖水体的表层水及沉积物中典型抗生素的残留分析[J].农业环境科学学报,2011(12):2586-2593.
[9] 王敏;俞慎;洪有为;孙棣棣.5种典型滨海养殖水体中多种类抗生素的残留特性[J].生态环境学报,2011(5):934-939.
[10] Pastor-Navarro N;Gallego-Iglesias E;Maquieira A.[J].TALANTA,200771(02):923.
[11] Cannavan A.;Blanchflower WJ.;Kennedy DG.;Hewitt SA..GAS CHROMATOGRAPHIC MASS SPECTROMETRIC DETERMINATION OF SULFAMETHAZINE IN ANIMAL TISSUES USING A METHYL/TRIMETHYLSILYL DERIVATIVE[J].The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry,199610(10):1457-1461.
[12] 周爱霞;苏小四;高松;张玉玲;林学钰;张兰英;安永磊.高效液相色谱测定地下水、土壤及粪便中4种磺胺类抗生素[J].分析化学,2014(3):397-402.
[13] Kung T A;Tsai C W;Ku B C.[J].Food Chemistry,2015175:189.
[14] Ebrahimpour B;Yamini Y;Rezazadeh M.[J].Environmental Monitoring and Assessment,2015187(01):4162.
[15] Natalia A M;Laura G G;Ana M G C.[J].Food Chemistry,2014143:459.
[16] Sun H;Ai L F;Wang F C.[J].CHROMATOGRAPHIA,200766(5/6):333.
[17] Nebot C;Regal P;Miranda M J.[J].Food Chemistry,2013141(03):2294.
[18] Marisol J B;Periche A;Donmenech E.[J].Food Con-trol,201550:243.
[19] 厉文辉;史亚利;高立红;刘杰民;蔡亚岐.加速溶剂萃取-高效液相色谱-串联质谱法同时检测鱼肉中喹诺酮、磺胺与大环内酯类抗生素[J].分析测试学报,2010(10):987-992.
[20] Huang X J;Chen L L;Yuan D X.[J].Analytical Biochemistry,2013405(21):6885.
[21] 杜玥;杨慧元;徐伟东.液相色谱-串联质谱法测定猪肉中23种磺胺及其增效剂残留[J].药物分析杂志,2010(3):471-478.
[22] 唐才明;黄秋鑫;余以义;彭先芝.高效液相色谱-串联质谱法对水环境中微量磺胺、大环内酯类抗生素、甲氧苄胺嘧啶与氯霉素的检测[J].分析测试学报,2009(8):909-913.
[23] 卢坤;童群义.高效液相色谱法同时检测蜂蜜中的5类抗生素残留[J].分析测试学报,2011(11):1320-1323,1328.
[24] 杨晓蕾;李杰;李学文;武虓.土壤中10种兽用抗生素的固相萃取-高效液相色谱-紫外测定法[J].环境与健康杂志,2012(4):357-360.
[25] 刘海新.柱后衍生法检测鳗鱼肌肉中磺胺类药物残留量研究[J].食品科学,2009(02):204-207.
[26] 李学德;鲜啟明;刘红玲;花日茂;许珊珊;陈海燕;于红霞.高效液相色谱-荧光检测法同时测定蔬菜中3种磺胺类药物残留[J].分析化学,2010(3):429-433.
[27] 黄冬梅;黄宣运;顾润润;惠芸华;田良良;冯兵;张璇;于慧娟.柱后衍生高效液相色谱法测定虾中14种磺胺类药物残留量[J].色谱,2014(8):874-879.
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