南京农业大学学报2017，Vol.40Issue(4)：703-709,7.DOI:10.7685/jnau.201612026
鸡蛋中硫酸头孢喹肟残留的高效液相色谱检测方法的建立
Establishment of high performance liquid chromatography method for measuring cefquinome sulfate residues in eggs
摘要
Abstract
[Objectives]To understand the elimination distribution of residue and the determination of the withdrawal time of cefquinome sulfate in eggs,the detection method of high performance liquid chromatography(HPLC) was established.[Methods]The samples were made by adding cefquinome sulfate into blank eggs according to the quality and volume proportion at 1:19.After being mixed totally,the cefquinome sulfate was extracted from eggs by acidic acetonitrile solution(adding 50 μL formic acid into 100 mL solution contented with 10 mL acetonitrile),mixing up totally for three times.After being degreased in n-hexane for 30 minutes,the extract solution was cleaned up on C18solid-phase extraction cartridges.The eluent was collected and dried under nitrogen evaporator in 40 ℃ water,and the residues were dissolved in mobile phase.The analyte was detected by high performance liquid chromatography(HPLC),under UV absorptive spectroscopy detector at 270 nm,after being filtered by microporous membrane.[Results]The testing data showed that the calibration curve was linearity at a range of 0.02-2.00 μg· mL-1,with a correlation coefficient(R2) of 0.999 8,which showed good linear relationship,the linear regression equation:y =164.95x+0.693.By comparing the S/N value,the lowcst limit of detection (LOD)was 0.01 μg·mL-1,and the lowest limit of quantitation (LOQ)was 0.02 μg· mL-1 for cefquinome sulfate in the tested eggs,respectively.With the concentrations of cefquinome sulfate at 0.01,0.10 and 1.00 μg· mL-1,the average recoveries were ranged from 85.6％ to 90.4％,and the coefficient of variances were ranged from 6.59％ to 10.47％,which were all within the prescribed scope.Meanwhile,this method was a specific,sensitive and rapid method for detecting the cefquinome sulfate residue in eggs.The results of stability test showed that,the samples under room temperature,4 ℃ (cold storage)and-20 ℃ (frozen)were stable within 24 hours,and the interference of clinical commonly used antimicrobial agents was not affected,which could meet the requirement of residue analysis.[Conclusions]With comprehensive analysis on all the testing data,the HPLC method established in this paper is conformed to the requirements of the adaptability and accuracy of residue detection.Meanwhile,this method can also be used in the detection of the cefquinome sulfate in eggs.关键词
硫酸头孢喹肟/鸡蛋/HPLC/残留检测Key words
cefquinome sulfate/egg/HPLC/assey of residue分类
农业科技引用本文复制引用
赵婕,李巧宁,刘爱玲,孟小宾,鲍恩东..鸡蛋中硫酸头孢喹肟残留的高效液相色谱检测方法的建立[J].南京农业大学学报,2017,40(4):703-709,7.基金项目
江苏高校优势学科建设工程资助项目(PAPD) （PAPD）
校企横向合作项目 （）
