摘要
目的 建立饮用水中23种抗生素同时测定的方法。方法 取经0.45μm玻璃纤维滤膜过滤后的1 L水样,调节p H值至2.0,加入内标物和Na2EDTA混匀,用HLB固相萃取小柱富集净化,甲醇洗脱,洗脱液浓缩后超高相液相色谱串联质谱法测定分析。结果 23种抗生素在0.5~50.0 ng/mL范围内线性关系较好(r≥0.99),检测限在0.01~0.35 ng/L,定量限为0.04~1.16 ng/L。低、中、高3种浓度的加标回收率为54.7%~114.3%,相对标准偏差为1.69%~12.38%。采用所建立的方法在源水和出厂水中检出了部分抗生素。结论 该方法操作简便、检测时间短、准确度和精密度较高,适用于源水和自来水中多种抗生素的测定。
Objective To establish a method for the simultaneous determination of 23 antibiotics in drinking water. Methods 1 L water sample filtered by 0.45 μm glass fiber filter membrane was taken,adjusting the pH to 2.0,the internal standard and Na2EDTA were added and mixed,concentrated and purified by an oasis HLB solid phase extraction column,with elution by methanol,and the eluent was concentrated and measured by the ultra-performance liquid chromatography-tandem mass spectrometry. Results The good linearity was obtained when the concentration of the 23 antibiotics were within 0.5-50.0 ng/mL(r ≥0.99),the limits of determination was 0.01-0.35 ng/L,and the limits of quantification was 0.04-1.16 ng/L.The recovery of samples was in the range of 54.7%-114.3% at 3 spike levels(low,medium and high). The relative standard deviations were in the range of 1.69%-12.38%.Some antibiotics were detected in source water and tap water by the established method. Conclusion The method has the advantages of simple operation,short detection time,high accuracy and precision,which is suitable for the determination of antibiotics in source water and tap water.
作者
纪律
万正杨
薛刚
杨财平
李琴娜
杨小波
JI Lyu;WAN Zheng-yang;XUE Gang;YANG Cai-ping;LI Qin-na;YANG Xiao-bo(Health Laboratory,Yichang Center for Disease Control and Prevention,Yichang Hubei,443005,China;Yichang Angel Yeast Testing Center,YichangHubei,443001,China)
出处
《职业与健康》
CAS
2022年第24期3360-3364,共5页
Occupation and Health
基金
湖北省教育厅科学技术研究项目(B2019017)
宜昌市医疗卫生研究项目(A20-2-053)。
关键词
抗生素
超高效液相色谱-串联质谱
固相萃取
Antibiotics
Ultra performance liquid chromatography-tandem mass spectrometry
Solid phase extraction
