刊名 |
Agricultural Biotechnology |
作者 |
Dandan LIU;Qing LI;Yaohong LIU;Sha FENG;Tao MO;Zheng LIU;Xiaonan ZOU |
作者单位 |
1. Guangzhou GRG Metrology & Test (Hunan) Co., Ltd., Changsha 410007, China; 2. Anhua Administration for Market Regulation, Yiyang 413500, China; 3. Guizhou Engineering Vocational College, Tongren 565200, China |
DOI |
DOI:10.19759/j.cnki.2164-4993.2024.01.016 |
年份 |
2024 |
刊期 |
1 |
页码 |
66-70,73 |
关键词 |
Landfill; Endocrine disruptor; Solid phase extraction; High performance liquid chromatography-tandem mass spectrometry |
摘要 |
[Objectives] This study was conducted to explore the occurrence levels of endocrine disruptors (EDCs) in rural areas around a county landfill in Tongren City. [Methods] The water around the landfill was sampled and analyzed. A solid-phase extraction and high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) method was established for the determination of 27 EDCs. After the HLB solid-phase extraction column was activated, 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 (100×2.1 mm, 2.6 µm) chromatographic column was adopted for LC separation by gradient elution with pure water 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 quantitation in the method were between 0.05 and 2.00 ng/L, and the recoveries ranged from 75.3% to 105.7%. [Conclusions] The method has high sensitivity, good accuracy and strong practical value. |