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| Determination of Dapsone and Its Metabolites in Aquatic Products by Solid Phase Extraction with High Performance Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） dapsone N-acetyl dapsone MCX solid phase extraction aquatic products |
| Author | Institution |
| WU Zi，HUANG Dong-mei，LOU Xiao-yi，ZHENG Rong，TANG Yun-yu，ZHANG Xuan，ZHANG Jun |
1. Key Laboratory of Control of Quality and Safety for Aquatic Products（Shanghai），Fishery Products Quality Inspection and Test Center （Shanghai），Ministry of Agriculture and Rural Affairs，East China Sea Fisheries Research Institute，Chinese Academy of Fishery Sciences，Shanghai ，China; 2. School of Food Science，Shanghai Ocean University，Shanghai ，China; 3. Ti Testing and Certification Group Co.，Ltd.，Shanghai ，China |
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| Abstract: |
| It is of great significance to develop novel analysis techniques for simultaneous determination of dapsone and its metabolites in aquatic products，so as to realize the simultaneous supervision of dapsone and its metabolites in aquatic products and the comprehensive control of illegal drug use．In this study，a high performance liquid chromatography－tandem triple quadrupole mass spectrometric（HPLC－MS/MS） method was established for the determination of dapsone and its metabolite residues in aquatic products．In the process of sample pre-treatment，the samples were extracted by using 10 mL 1% ammoniated acetonitrile with dapsone-D8 as the internal standard，followed by fat removal with n-hexane．Meanwhile，MCX cationic solid phase extraction column was used for enrichment and purification．The eluent was concentrated to about 0.2 mL by nitrogen blowing at 45 ℃，and then fixed with 10% methanol solution to 1 mL．After mixing，the eluent was filtered through a 0.22 μm aqueous phase membrane into an injection vial for detection by HPLC－MS/MS．The separation was carried out on a CAPCELL PAK C18（2.0 mm × 100 mm，3 μm） by gradient elution using methanol－water as mobile phases．The quantitative analysis of target compounds was performed by the internal standard method under multiple reaction monitoring（MRM） and positive ion ionization modes．The results showed that the calibration curves for dapsone and N-acetyl dapsone were linear in the mass concentration range of 0.1－5.0 μg/kg，with correlation coefficients（r2） all greater than 0.99．The limits of detection（LODs） were 0.1 μg/kg and the limits of quantitation（LOQs） were 0.2 μg/kg．The average recoveries at three spiked levels of 0.2，1.0，2.0 μg/kg ranged from 94.0% to 109%，with relative standard deviations（RSDs） of 2.7%－11%．The positive muscle samples obtained in the drug substitution experiment were determined，and the metabolite of dapsone was identified as N-acetyl dapsone by identifying the retention time of the compound and the ion pair information．This method has low detection limit，good precision and high accuracy，which could realize the accurate qualitative and quantitative determination of dapsone residues in fish，shrimp，crab，shellfish and other aquatic products． |
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