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| Determination of Diazepam and Its Metabolites in Aquaculture Environment Samples by Solid Phase Extraction Cleanup and Ultra-performance Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:diazepam metabolite solid phase extraction（SPE） ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS） aquaculture environment |
| Author | Institution |
| WANG Xu-feng，WANG Qiang，ZHANG Ying-xia，HUANG Ke |
South China Sea Fisheries Research Institute，Chinese Academy of Fishery Sciences，Fishery Environment and Aquatic Products Quality Inspection & Testing Center of the Ministry of Agriculture and Rural Affaires（Guangzhou），Guangzhou ，China |
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| Abstract: |
| A multi-residue analytical method was developed for the simultaneous determination of diazepam and its three metabolites in aquaculture water and sediment samples based on ultra-performance liquid chromatography－tandem mass spectrometry（UPLC－MS/MS）．Water samples were filtered through 0.45 μm glass fiber membranes，and subsequently enriched with a mixed cation exchange solid phase extraction（MCX SPE） cartridge．Sediment samples were extracted with 1% ammonium hydroxide－ethyl acetate，and then cleaned up using a MCX SPE cartridge．The purified extracts were eluted with 5% ammonium hydroxide－acetonitrile solution，and then dried residues were redissolved with 1 mL 40% acetonitrile water solution for UPLC－MS/MS analysis．The chromatographic separation of four targeted analytes were performed on a Phenomenex Kinetex C18（100 mm × 2.1 mm，1.7 μm） column by gradient elution，with acetonitrile and 0.1% formic acid solution as mobile phases．Targeted compounds were determined with positive electrospray ionization under multiple reaction monitoring（MRM） mode，and quantified by internal standard method．Good linear relationships for targeted analytes were obtained in the range of 0.1－100 μg/L with correlation coefficients（r2） larger than 0.999．The detection limits of the method for aquaculture water samples and sediment samples were 1.0－2.0 ng/L and 0.02－0.05 μg/kg，while the quantitation limits were 2.0－5.0 ng/L and 0.05－0.1 μg/kg，respectively．The average recoveries for spiked negative aquaculture water and spiked sediment matrix ranged from 90.2% to 115%，with relative standard deviations（RSDs，n = 6） between 2.1% and 9.6%．The proposed method is sensitive and accurate，and it is suitable for the residual determination of diazepam and its metabolites in real aquaculture water and sediment samples. |
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