李金玲, 杨愿愿, 刘思思, 赵建亮, 应光国, 陈长二. 水样中5种氟喹诺酮的UPLC-QTOF法测定[J]. 华南师范大学学报(自然科学版), 2021, 53(2): 44-50. doi: 10.6054/j.jscnun.2021025
引用本文: 李金玲, 杨愿愿, 刘思思, 赵建亮, 应光国, 陈长二. 水样中5种氟喹诺酮的UPLC-QTOF法测定[J]. 华南师范大学学报(自然科学版), 2021, 53(2): 44-50. doi: 10.6054/j.jscnun.2021025
LI Jinling, YANG Yuanyuan, LIU Sisi, ZHAO Jianliang, YING Guangguo, CHEN Changer. Determining Five Fluoroquinolone Antibiotics in Water Samples with the UPLC-QTOF Method[J]. Journal of South China Normal University (Natural Science Edition), 2021, 53(2): 44-50. doi: 10.6054/j.jscnun.2021025
Citation: LI Jinling, YANG Yuanyuan, LIU Sisi, ZHAO Jianliang, YING Guangguo, CHEN Changer. Determining Five Fluoroquinolone Antibiotics in Water Samples with the UPLC-QTOF Method[J]. Journal of South China Normal University (Natural Science Edition), 2021, 53(2): 44-50. doi: 10.6054/j.jscnun.2021025

水样中5种氟喹诺酮的UPLC-QTOF法测定

Determining Five Fluoroquinolone Antibiotics in Water Samples with the UPLC-QTOF Method

  • 摘要: 建立了环丙沙星、恩诺沙星、诺氟沙星、氧氟沙星和培氟沙星等5种氟喹诺酮类抗生素(FQs)的超高效液相色谱-四极杆飞行时间质谱(UPLC-QTOF)定量分析方法. 样品经Waters ACUITY UPLC BEH C18色谱柱分离,含0.1%甲酸(体积分数)的水溶液-甲醇为流动相进行梯度洗脱,电喷雾串联飞行时间质谱正离子模式扫描,分别在UPLC-QTOF的MS、MSE和多反应监测(MRM)模式进行检测,采用内标法定量,并与超高效液相色谱-三重四极杆质谱(UPLC-TQMS)的MRM模式进行比较研究. 结果表明:UPLC-QTOF测定的检出限为0.04~0.22 μg/L,定量限为0.17~0.90 μg/L,且在1~100 μg/L范围内,表现了良好的线性关系(R2≥0.99),该方法各项指标及环境样品应用与UPLC-TQMS法相当. 因此,UPLC-QTOF可对水环境样品中这5种FQs进行筛查和定量分析.

     

    Abstract: A quantitative method was developed for the simultaneous determination of five fluoroquinolones (FQs), including ciprofloxacin, enrofloxacin, norfloxacin, ofloxacin and pefloxacin, using ultra performance liquid chromatography-quadruple time of flight mass spectrometry (UPLC-QTOF). Samples were separated on Waters ACUITY UPLC BEH C18 column with gradient elution programs, using methanol and water containing 0.1% formic acid as the mobile phases, and analyzed in electrospray positive ion source, using three acquisition modes (MS, MSE and MRM). Five FQs were quantified with an internal standard method. Limits of detection (LOD) and limits of quantification (LOQ) of the 5 FQs on the UPLC-QTOF were 0.04~0.22 μg/L and 0.17~0.90 μg/L, respectively. Linear ranges of the 5 FQs were 1~100 μg/L with good correlation coefficients (R2≥0.99). This method was compared with the UPLC-tandem mass spectrometry (UPLC-TQMS) method and showed comparable performance. UPLC-QTOF is fast, sensitive, and suitable for the simultaneous quantification of the 5 FQs in environmental water samples.

     

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