FENG Yue-chao,DING Qi,YANG Yi-fan,et al.Fully Automated Online Solid Phase Extraction-Super High Performance Liquid Chromatography – Tandem Mass Spectrometry Determination of 15 Quinolones in Reclaimed Water[J].China Water & Wastewater,2020,36(12):143-149.
Fully Automated Online Solid Phase Extraction-Super High Performance Liquid Chromatography – Tandem Mass Spectrometry Determination of 15 Quinolones in Reclaimed Water
- Keywords:
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reclaimed water
; quinolones; online solid phase extraction; super high performance font-size: 10pt; ">liquid chromatography-tandem mass spectrometry
- Abstract:
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A fully automated online solid phase extraction-super high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS)method was developed for detecting 15 quinolones in reclaimed water samples. The samples were acidized with 0.2%formic acid, then added 5% methanol. The injection volume was 5 mL, and the instrument automatically completed 6 steps: loading sample, cleanup, elution, online SPE column regeneration, separation of the object and determination by mass spectrometry. The analytical methods were electrospray positive ion scanning (ESI +), multi-reaction monitoring (MRM) mode detection, and external standard legal quantity. When the standard concentration range was 0.05-5 μg/L, the standard curve of 15 quinolones was linear and the correlation coefficient (R2) was greater than 0.991. The recovery range was 84.4%-116.2%(n=6), the RSD was no more than 19.92%, and the limit of detection (LOD) range was 0.7-8.7 ng/L. 30 reclaimed water samples were analyzed by this method. As a result, 7 quinolones were detected in 13 reclaimed water samples. The concentration of the compounds ranged from 0.004 2 to 0.47 μg/L.