电膜萃取/高效液相色谱法检测生物样品中3种喹诺酮类抗生素  

Determination of Three Quinolone Antibiotics in Biological Samples by High Performance Liquid Chromatography Coupled with Electromembrane Extraction

作　　者：伏广想 张婷[1] 彭俞霖 吕荫妮[1] FU Guang-xiang;ZHANG Ting;PENG Yu-lin;LÜYin-ni(College of Criminal Science and Technology,Criminal Investigation Police University of China,Shenyang 110854,China)

机构地区：[1]中国刑事警察学院刑事科学技术学院,辽宁沈阳110854

出　　处：《分析测试学报》2024年第9期1467-1473,共7页Journal of Instrumental Analysis

基　　金：辽宁省教育厅面上科研项目(2021LJKZ0070);辽宁省法庭科学重点实验室开放课题(FTKX2022KF02)。

摘　　要：建立了电膜萃取(EME)结合高效液相色谱(HPLC)快速测定尿液和鱼肉组织中左氧氟沙星、诺氟沙星、环丙沙星3种喹诺酮类抗生素的分析方法。将尿液稀释,鱼肉研碎后用pH 5.0的磷酸盐缓冲液稀释作为供体相,随后进行EME。确定药物萃取的接收相溶液为pH 2.0的10 mmol/L盐酸,萃取电压为35~70 V,萃取时间为20 min,采用HPLC检测。结果表明,尿液和鱼肉中3种喹诺酮类抗生素在各自质量浓度范围内线性关系良好,相关系数(r^(2))均大于0.99;尿液中药物的检出限和定量下限分别为2.0~5.2 ng/mL和6.8~17.6 ng/mL,鱼肉中的检出限和定量下限分别为12~36 ng/g和42~121 ng/g。在3个不同浓度加标水平下,尿液与鱼肉基质中喹诺酮类抗生素的加标回收率为67.7%~127%,相对标准偏差(RSD,n=6)为4.2%~10%。该方法前处理操作简单、有机试剂用量少、净化效果和重复性好,可满足尿液和鱼肉中3种喹诺酮类抗生素的检测需求。An analytical method was developed for the rapid determination of three quinolone antibi⁃otics in urine and fish tissues by electromembrane extraction(EME)coupled with high performance liquid chromatography(HPLC).The urine was diluted,and the fish meat was minced and extracted with pH 5.0 phosphate buffer,followed by EME.The receiving solvent for drug extraction was deter⁃mined to be 10 mmol/L hydrochloric acid at pH 2.0,extraction voltage of 35-70 V,extraction time of 20 min,and HPLC detection.Results showed that the three quinolone antibiotics in urine and fish meat showed good linearity in their respective mass concentration ranges with correlation coefficients(r^(2))greater than 0.99.The limits of detection and limits of quantification of the drugs ranged from 2.0 to 5.2 ng/mL and from 6.8 to 17.6 ng/mL in urine and from 12 to 36 ng/g and from 42 to 121 ng/g in fish,respectively.The recoveries of quinolone antibiotics in urine and fish matrix spiked at three different concentration levels were 67.7%-127%with the relative standard deviations(RSDs,n=6)of 4.2%-10%.The pretreatment method is simple,with low dosage of organic reagents,good pu⁃rification effect and reproducibility,and can meet the requirements for the determination of the three quinolone antibiotics in urine and fish.

关 键 词：喹诺酮 电膜萃取 高效液相色谱 尿液 鱼肉 抗生素 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]