高效液相色谱-串联质谱法测定蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑  

Determination of residues of chloramphenicol, thiamphenicol, florfenicol and metronidazole in Honey by HPLC-MS/MS

作　　者：李潇舟 陈海平[1] LI Xiao-zhou;CHEN Hai-ping(Haidian District Center for Disease Control and Prevention,Beijing 100094,China)

机构地区：[1]北京市海淀区疾病预防控制中心,北京100094

出　　处：《现代预防医学》2022年第13期2420-2425,共6页Modern Preventive Medicine

摘　　要：目的建立蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑残留的高效液相色谱-串联质谱同时测定方法。方法以乙酸乙酯作为提取剂,经涡旋混匀提取后,氮吹至干,用5%甲醇水溶解,Oasis HLB固相萃取柱净化。经甲醇洗脱,洗脱液经45℃水浴氮吹至干,流动相涡旋溶解,上机测定。高效液相色谱分离、串联质谱检测,采用多离子反应监测(MRM)模式,内标法定量。结果在优化条件下,4种抗生素浓度在0.1~5.0μg/L范围内,线性关系良好,相关系数(r)≥0.9953,方法检出限≤0.015μg/kg,不同基质中平均加标回收率为78.5%~95.1%,相对标准偏差(RSD)为2.8%~10.7%。结论该方法快速、灵敏、准确,适用于蜂蜜中氯霉素、甲砜霉素、氟甲砜霉素及甲硝唑的同时测定。Objective To establish a method for simultaneous determination of chloramphenicol,thiamphenicol,florfenicol and metronidazole residues in honey by high-performance liquid chromatography-tandem mass spectrometric method(HPLC-MS/MS).Methods The residue was extracted by vortex mixing,which used ethyl acetate as extractant,then dried-up under nitrogen flow,and dissolved in 5%methanol-water.The sample solution was purified with Oasis HLB solid phase extraction column.After elution with methanol,the eluent was blown to dryness under nitrogen flow in water bath at 45℃.The residue was dissolved in mobile phase by vortex,and separated by using HPLC and detected by MS/MS in positive and negative ion multiple reaction monitoring(MRM)mode.The quantifications were based on internal standard method.Results Under the optimized conditions,the calibration curves for the 4 antibiotics were linear in the range of 0.1-5.0μg/L with the correlation coefficients(r)of≥0.9953,and the limit of detection was 0.015μg/kg.The average recovery rates of 4 antibiotics residues from different matrices were within 78.5%-95.1%,and the relative standard deviations(RSD)range were 2.8%-10.7%.Conclusion The method is effective,sensitive,and accurate.It can be used to simultaneously determine the residues of chloramphenicol,thiamphenicol,florfenicol and metronidazole in honey.

关 键 词：抗生素 蜂蜜 固相萃取 高效液相色谱-串联质谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]