| 张凯,公维磊,倪永付,刘杰锋,慕明伟.HPLC-MS/MS法测定济宁市区河水中4种喹诺酮类抗生素残留[J].济宁医学院学报,2018,41(4):264-267 |
| HPLC-MS/MS法测定济宁市区河水中4种喹诺酮类抗生素残留 |
| Determination of 4 kinds of common quinolone antibiotics in the river water of Jining urban area by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2017-11-27 |
| DOI：10.3969/j.issn.1000-9760.2018.04.010 |
| 中文关键词: 固相萃取;高效液相色谱-串联质谱;喹诺酮类抗生素 |
| 英文关键词: Solid phase extraction;High performance liquid chromatography-tandem mass spectrometry;Quinolone antibiotics |
| 基金项目: |
| 作者 | 单位 | | 张凯 | 济宁医学院法医学与医学检验学院, 济宁 272067 | | 公维磊 | 济宁医学院法医学与医学检验学院, 济宁 272067 | | 倪永付 | 济宁出入境检验检疫局, 济宁 272000 | | 刘杰锋 | 济宁医学院, 济宁 272067 | | 慕明伟 | 济宁医学院, 济宁 272067 |
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| 中文摘要: |
| 目的 采用高效液相色谱-串联质谱（HPLC-MS/MS）法测定济宁市区河水中诺司帕沙星、洛美沙星、萘啶酸、氟甲喹4种喹诺酮类抗生素，以探索济宁市区河水中喹诺酮类抗生素的污染现状。方法 采集的水样经HLB固相萃取柱富集，真空干燥后，先用0.5%甲醇淋洗再用甲醇洗脱，氮吹浓缩至0.1ml以下，最后用0.1%甲醇定容至0.5ml，以0.1%甲酸水-乙腈为流动相上机检测。采用Hypersil GOLD-1.9μm，50mm×2.1mm （i.d）色谱柱分离，在电喷雾离子源（electrospray ion source，ESI）、正离子模式、多重反应监测（multi-reaction monitoring，MRM）模式下测定，外标法定量。结果 所测4种喹诺酮类化合物均在浓度为5~200μg/L的线性范围内，线性关系良好，相关系数R2均>0.99，回收率81.9%~115.0%，相对标准偏差均<10%，定量限为10μg/L，市区河水所采集的20个样品未检出司帕沙星、洛美沙星、萘啶酸，但均检出氟甲喹，且均低于定量限10μg/L。结论 济宁市区河水中诺司帕沙星、洛美沙星、萘啶酸在检出限内均未检出，所有水样均检测出氟甲喹，含量较低，但应引起有关部门注意，观察长期效应。 |
| 英文摘要: |
| Objective To determine four kinds of quinolone antibiotics,including nobsparfloxacin,lomefloxacin,naphthalic and flumequine in the river water of Jining urban area by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry,in order to explore the river water pollution status of quinolone antibiotics in the area.Methods Water samples were enriched by HLB solid phase extraction column.After vacuum drying,the samples were eluted with 0.5% methanol and then with methanol.The samples were concentrated to 0.1 ml or less by organomation,and finally diluted with 0.1% methanol to 0.5 ml.The solution of formic acid water-acetonitrile was used as mobile phase on the machine detection.The samples were separated by Hypersil GOLD-1.9μm,50mm×2.1mm (id),and determined in the mode of electerspray ion source (ESI),positive ion mode,multi-reaction monitoring (MRM) mode,and quantified by external standard method.Results The 4 kinds of quinolone antibiotics had good linear relation (R2>0.99) at the range of 5μg/L~200μg/L.The recoveries were in the range of 81.9%~115.0%.The relative standard deviations were less than 10% and the limit of quantification was 10μg/L.Nobsparfloxacin,lomefloxacin and naphthalic were not detected in the 20 samples collected from the urban river.However,flumequine was detected in all samples,but the concentrations were below 10μg/L.Conclusion Nobsparfloxacin,lomefloxacin and naphthalic in the river water of Jining urban area were not detected within the detection limit.Flumequine was detected with low concentration in all water samples.The results suggested that the relevant departments should pay more attention to observe the long-term effect of flumequine in the river water of Jining urban area. |
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