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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: To establish a method for simultaneous determination of trace residues of 28 antibiotics in honey by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). Methods: The samples were purified by solid-phase extraction and separated by reversed-phase liquid chromatography. Testing is done in multiple reaction monitoring mode (MRM). Quantitative analysis based on retention time, precursor ions and signature ion information. Results: Among the 28 antibiotics, lincomycin hydrochloride, clindamycin hydrochloride, fleroxacin, sulfadiazine, sulfamethazine, sulfamidine, sulfamethoxazole, sulfamethoxazole, ciprofloxacin, Tetracycline, tetracycline, tetracycline, tetracycline, tetracycline, tetracycline, tetracyclines The limit of detection (LOD) and the limit of quantitation (LOQ) of roxithromycin and roxithromycin were 0.5μg · kg-1 and 1.25 ~ 200ng · mL-1, respectively. (R2> 0.99); the detection limit of sulfanilamide, penicillin sodium, penicillin V potassium, tetracycline hydrochloride, doxycycline hyclate, chlortetracycline hydrochloride and 4-epi-chlortetracycline was 0.5μg · kg- The limit was 1.0μg · kg-1, with a good linear relationship (R2> 0.99) in the range of 1.25 ~ 200ng · mL-1. In the study, spiked recoveries of 1.0 μg · kg-1, 4.0 μg · kg-1 and 20.0 μg · kg-13 were selected. The results of external standard method and the average recoveries of three levels were satisfactory. Intraday precision of less than 8% (n = 5), daytime precision of less than 10% (n = 5), to meet the needs of routine analysis. Conclusion: The method is rapid, sensitive and accurate and is suitable for the simultaneous determination of trace residues of many antibiotics in honey.