摘要
目的:建立了固相萃取-高效液相色谱-串联质谱(HPLC-MS/MS)法同时定量检测蜂蜜中28种抗生素药物的痕量残留。方法:样品经固相萃取提取净化、反相液相色谱分离后进行质谱分析。在多反应监测模式(MRM)下进行检测。根据保留时间、母离子和特征子离子信息进行定量分析。结果:28种抗生素药物中盐酸林可霉素、盐酸克林霉素、氟罗沙星、磺胺嘧啶、磺胺二甲嘧啶、磺胺脒、磺胺氯哒嗪、磺胺甲恶唑、环丙沙星、诺氟沙星、洛美沙星、依诺沙星、巴洛沙星、司帕沙星、甲磺酸培氟沙星、氧氟沙星、甲硝唑、替硝唑、4-差向四环素、土霉素、罗红霉素的检出限(LOD)为0.2μg·kg-1,定量限(LOQ)为0.5μg·kg-1,在1.25～200ng·mL-1范围内,均呈良好线性关系(R2>0.99);磺胺、青霉素钠、青霉素V钾、盐酸四环素、盐酸多西环素、盐酸金霉素、4-差向金霉素的检出限为0.5μg·kg-1,定量限为1.0μg·kg-1,在1.25～200ng·mL-1范围内,均呈良好线性关系(R2>0.99)。研究选择1.0μg·kg-1,4.0μg·kg-1,20.0μg·kg-13个添加浓度水平进行加标回收试验,外标法定量,3个水平的平均回收率结果均令人满意。日内精密度小于8%(n=5),日间精密度小于10%(n=5),满足日常分析的需要。结论:该方法快速、灵敏、准确,适用于同时检测蜂蜜中多种抗生素类药物的痕量残留。
Objective： It has been developed an high - performance liquid chromatography - tandem mass spectrometry（LC- MS/MS） method for the simultaneous determination of twenty -eight antibiotics residues in honey. Method ： A solid - phase extraction was employed in the preparation procedure. The residues of antibiotics were analyzed by reversed - phase high performance liquid chromatography （ RP - HPLC ） coupled with electrospray tandem mass spectrometry. Multiple reaction monitoring（MRM） mode was employed for the quantitative determination. The chromatographic separation was performed on an Agilent ZORBAX Eclipse Plus C18 column （150 mm× 2. 1 mm, 3.5 μm）. Results： The limits of detect （ LOD ） about lincomycin hydrochloride, clindamycin hydrochloride, fleroxacin, sulfamethoxazole, sulfadimidine, sulfaguanidine, sulfachloropyridazine, sulfamethoxazole, ciprofloxacin, norfloxacin, lomefloxaein, enoxacin, balofloxacin, sparfloxacin, pefloxacin, ofloxacin, metronidazole, tinidazole,4- chatetracycline hydrochloride, oxytetracycline hydrochloride ,roxithromycin was 0. 2 μg·kg^-1, the limits of quantification （LOQ）was 0. 5 μg·kg^-1 ; the linear ranges were between 1.25and 200 ng · mL^-1 , and R^2 〉0.99. The limits of detect （LOD） about sulfanilamide, benzylpenicilinsodium, phenoxymethyl penicillin potassium, tetracycline hydrochloride, doxycycline hydate, chlortetracycline hydroehloride, 4 -cha chlortetracycline hydrochloride was 0. 5 μg · kg^-1, the limits of quantification （LOQ）was 1.0 μg· kg^-1, the linear ranges were obtained between 1.25 and 200 ng · mL^-1 , and R2 〉 0.99. The average spiking recoveries of 28 antibiotics were ranged from 70% to 110% , with relative standard deviations between 1.0% and 10. 0%. Intra - day and inter - day variations of the method were all within the acceptable ranges. Conclusion ：The method is rapid, sensitive,accurate, simple and suitable for the identification and quantification of these antibiotics residues in honey.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第7期1196-1201,共6页
Chinese Journal of Pharmaceutical Analysis
基金
天津市食品药品监督管理局局级课题
关键词
液相色谱-串联质谱
固相萃取
抗生素类药物
残留
蜂蜜
liquid chromatography mass spectrometry
solid - phase extraction
antibiotics
residues
honey
