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| Determination of 9 Kinds of Banned Dye Drugs in Aquatic Products by High Performance Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） banned dyes drugs aquatic products |
| Author | Institution |
| SUN Liang-juan，LI Hong-quan，CAI Run-bin，ZHUANG Jiang-yun，TANG Qing-qiang，TANG Yuan-yuan，ZHONG Jian，HUANG Wu |
1. Zhanjiang Customs Technology Center，Zhanjiang ，China; 2. Fuzhou Customs Technology Center，Fuzhou ，China |
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| Abstract: |
| A high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） method was developed for the determination of nine banned dyes in aquatic products，including bright green，methylene blue and its three metabolites，malachite green and leucomalachite green，crystal violet and leucocrystal violet．After pretreatment procedure，samples were extracted with acetonitrile－0.1 mol/L ammonium acetate（pH 4.5） solution．Extract solution were purified by salt-out extraction of sodium chloride，n-hexane and PRS solid phase extraction column．The targets were separated on a Luna C18（2.1 mm × 50 mm，5 μm） column with a mobile phase consisting of acetonitrile-5 mmol/L ammonium acetate（0.1% formic acid） for gradient elution．Mass spectrometry multiple reaction monitoring（MRM） and positive ion ionization mode were used for testing and external standard method was used for quantitative analysis．Good linear relationships were obtained for nine compounds in the content range of 0.5－20.0 μg/L，with correlation coefficients（r2） greater than 0.99．The limits of detection（LODs）were 0.5 μg/kg，and limits of quantitation（LOQs）were 1.0 μg/kg．Tilapia，pomfret，shrimp and crab were used as the blank matrix，and spiked at the levels of 0.5，1.0，5.0 μg/kg．The average recoveries were 76.8%－104%，and the relative standard deviations（RSDs，n = 7） were 4.3%－10%．By using this method，methylene blue and azure B were detected in tilapia samples which were treated with methylene blue medicine bath．The method is accurate，reliable and reproducible，so it can be used for the quantitative analysis of 9 banned dyes in aquatic products. |
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