收稿日期: 2015-03-30
网络出版日期: 2017-06-30
基金资助
国家自然科学基金资助项目(41430644, 11175112, 41373098, 41273141, 41473090)
Determination of 12 antibiotics in aqueous environment by high performance LC-MS/MS
Received date: 2015-03-30
Online published: 2017-06-30
利用固相萃取(solid phase extraction, SPE)及液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)联用技术, 建立了水体中痕量磺胺类、β-内酰胺类、四环素类、喹诺酮类、大环内酯类等12 种抗生素的定量分析方法. 水样中的12 种抗生素通过亲水疏水平衡(hydrophile lipophilic balance, HLB)小柱的萃取富集后, 以乙腈为有机相、0.2% 甲酸和醋酸铵混合水溶液为水相, 采用LC-MS/MS 进行定量分析. 抗生素采用电喷雾电离(electrospray ionization, ESI)源多反应监测(multiple reaction monitoring, MRM)模式, 以13C3-caffeine 作为内标物进行定量检测. 抗生素在河水中的方法定量限为0.004 83~4.805 00 ng/L, 回收率为71%90%. 该方法被应用于分析南陈河(上海)中抗生素的含量, 平均质量浓度为2.04254.46 ng/L.
徐晖, 吴明红, 徐刚 . 高效液相色谱-串联质谱法对水环境中12种抗生素的检测[J]. 上海大学学报(自然科学版), 2017 , 23(3) : 483 -490 . DOI: 10.12066/j.issn.1007-2861.1655
This paper proposes a quantitative method for trace detection of 12 antibiotics including sulfonamides, β-lactams, fluoroquinolones, tetracyclines, macrolides in waters using solid phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS). After enriching thought hydrophile lipophilic balance (HLB) cartridges, 12 antibiotics are detected by LC-MS/MS with the organic phase of acetonitrile and aqueous phase of ammonium acetate and 0.2% formic acid. The antibiotics are quantified with multiple reaction monitoring (MRM) mode by internal standard of 13C3-caffeine. Quantification limits for antibiotics are from 0.004 83 to 4.805 00 ng/L in river water and the recoveries ranged from 71% to 90%. The method is applied to detect antibiotics in Nanchen River, Shanghai. Mean concentrations of antibiotics are from 2.04 to 254.46 ng/L.
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