HPLC法同时测定牛奶中7种磺胺类药物和4种氟喹诺酮类兽药  

Simultaneous determination of sulfonamides and fluoroquinolones residues in milk by high performance liquid chromatography

作　　者：邬晨阳[1] 韩小江[1] 

机构地区：[1]浙江省慈溪市疾病预防控制中心,浙江慈溪315300

出　　处：《中国卫生检验杂志》2011年第2期353-355,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的:建立了一种同时测定牛奶中两类共11种兽药(7种磺胺类药物和4种氟喹诺酮类药物)残留量的高效液相色谱分析。方法:样品经水-乙腈(V∶V=1∶1)提取,过C-18固相萃取柱净化,残余物用流动相定容至1 ml,以乙腈和磷酸二氢钾溶液作为流动相,采用梯度洗脱程序进行液相色谱分离,用紫外检测器进行定性和定量分析。结果:磺胺类药物和氟喹诺酮类药物在0μg/ml^50μg/ml范围均具有良好的线性,相关系数均大于0.999,检出限(S/N)分别为1.3和0.8μg/L,添加水平为30,4μg时,11种兽药的平均回收率分别为88.56%~91.65%和87.25%~91.57%,RSD均小于10%。结论:实验结果表明,该方法灵敏度高,重现性好,准确度高,可满足动物源性食品中磺胺和氟喹诺酮类药物的残留分析。Objective：A method was developed for the simultaneous determination of 11 residual antibiotics-seven sulfonamides and four fluoroquimolones in milk by high performance liquid chromatographyelectrospray.Methods： The sample was extracted with water –acetonitrile（V∶V=1∶1）.then purified by an C-18solid-phase extraction column.After evaporation,the residue was dissolved in the mobile phase of 1 ml.The HPLC separation was performed with a gradient elution program of acetonitrile and potassium dihydrogen phosphate as the molile phase.The identification and quantification were done with UV.Results： The linear range of the method was 0 μg/ml^200 μg/ml for SAs and FQs,both with correlation coefficients of more than 0.999,the limits of detection（S/N）were 1.3 μg/L for SAs and 0.8 μg/L for FQs respectively.At the spiked levels of 30 and 4 μg,the average recoveries for 11 residual antibiotics were 88.56%~91.65% and 87.25%~91.57%,both RSDs were less than 10%.Conclusion： The experimental results show that this method is of high sensitivity,good reproducibility,better determination capacity and shorter analysis time.The method can be used for the multi-residue analysis of sulfonamides and fluoroquinolones in milk foods.

关 键 词：高效液相色谱 磺胺 氟喹诺酮 动物源性食品 

分 类 号：O657.72[理学—分析化学]