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1、2005,14(1)水产品中四环素类抗生素残留量的高效液相色谱测定方法2093研究报告3水产品中四环素类抗生素残留量的高效液相色谱测定方法黄志勇,蔡洪基,黄高凌,彭爱红(集美大学生物工程学院,福建,厦门361021)摘要本文建立了高效液相色谱(HPLC)检测水产品中3种四环素类抗生素残留量的方法。采用4%高氯酸溶-1液提取样品中的残留抗生素,经浓缩处理,以乙氰和0.01mol·LNaH2PO4(18∶82,v/v)为流动相,流速-1-11mL·min,3种抗生素组分峰能与杂质峰完全分开,检测波长为355mm。在50~1000μg·m
2、L范围2内,峰面积与抗生素浓度呈良好的线性关系(r>0.99),以测量的3倍标准偏差计算方法的检出限分别-1-1-1为0.045μg·g(土霉素)、0.041μg·g(四环素)和0.080μg·g(金霉素)。平均加标加收率分别为96.5%(土霉素)、87%(四环素)和73.2(金霉素)。精密度(RSD)小于5%。实验检测了几种常见水产品样品的四环素类抗生素残留量,发现在本检出水平下被检测的几种鱼和虾样品均未能检出。关键词四环素类抗生素;残留;水产品;高效液相色谱Determinationoftetracyclineantibioti
3、cresiducsinaquiculturcproductsbyHPLCHuangZhiyong,CaiHongji,HuangGaoling,PengAihong(CollegeofBioengineering,JimeiUniversity,Xiamen,Fujian,361021)AbstractTheresiduesoftetracyclineantibioticsincludingoxytetracycline(OTC),tetracycline(TC)andchlortetracy2cline(CTC)inseveral
4、kindsofaquicultureproductsweremeasuredwiththeoptimizedmethodofhighperformanceliquidchromatography(HPLC).Thetetracyclineantibioticsinseafoodsampleswereextractedtwiceby4%HClO4,andthecom2binedextractswereconcentratedtilldrynessin70℃waterbathunderagentlestreamofnitrogen.Th
5、en,itsresiduewasre2solvedin4%HClO4andthesolutionswerefiltratedwith0.45μmmembrane.Thetetracyclineantibioticsamplesweresepa2-1ratedbytheRP-HPLCcolumn(Waters3.6mm×15cm,4.6μm)withamobilephaseofacetonitrileand0.01mol·LNaH2PO4(18∶82,v/v)attherateof1mL/minanddetectedat355nm.T
6、heaveragerecoveriestestedwithaddingstand2ardswere96.5%forOTC,87%forTCand73.2%forCTC,andthedetectionlimitestimatedwith3-foldstandarddevia2-1-1-1tionwas0.045μg·gforOTC,0.041μg·gforCTCand0.080μg·gforCTC,respectively.Thethreekindsoftetra2cyclineantibioticsinactualaquicultu
7、reproductscouldnotbedetectedwiththeestablishedmethod.KeywordsTetracyclineantibiotics;residue;Aquicultureproducts;Highperformanceliquidchromatography(HPLC)四环素类抗生素包括土霉素(oxytetracycline,品残留监控计划中对四环素类抗生素的残留量进[2]OTC)、四环素(tetracycline,TC)和金霉素(chlortet2行了严格的检测和限量控制。四环素类抗生素rac
8、ycline,CTC)等,属广普类抗生素药物,由于其具的残留检测有微生物法、酶联免疫法、紫外分光光有良好的杀菌或抑菌作用而广泛用了防治动物和度法、荧光光度法和薄层色谱法(TLC)等,其中微生[1]水产品的疾病感染。但动物源性食品中抗生