摘要
[Objectives] An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for simultaneous determination of 26 antibiotics in the water around landfills. [Methods] After an HLB solid-phase extraction column was activated, and a water sample, which was adjusted with phosphoric acid to a pH of (2±0.5) and added with 500 mg of disodium EDTA, was loaded, and 5 ml of water and 20% methanol water was added for washing. Next, 10 ml of elution solution was added for elution, and the collected eluate was evaporated under reduced pressure at 40 ℃ to near dryness, and 1 ml of reconstitution solution was added to a constant volume. An ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 2.6 μm) chromatographic column was adopted for LC separation by gradient elution with 0.1% formic acid aqueous solution-acetonitrile as the mobile phase. For MS detection, the MRM mode was adopted for collection, and the positive and negative ion modes were switched for simultaneous determination, and the internal standard method was used for quantification. [Results] The correlation coefficient R2 was greater than 0.99 in the linear range of each target substance. The limits of detection ranged from 0.15 to 3.00 ng/L, and the limits of quantitation were between 0.80 and 10.00 ng/L, and the recoveries ranged from 77.9% to 104.85%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value.
基金
Supported by Tongren Science and Technology Planning Project(TSKY[2022]42)
Science Planning Project of Department of Education of Guizhou Province(2023B111)。
