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液相色谱串联质谱法测定进出口水产品中亚甲基蓝药物残留.pdf

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Hans Journal of Food and Nutrition Science 食品与营养科学, 2012, *, **-** doi:***/hjfns.2012.*** Published Online *** 2012 (/journal/hjfns/) Determination of methylene blue drug residues in import and export aquatic products by liquid chromatography-tandem mass spectrometry 1 1 2 2 1 1 1 1 Juyi Yin , Jie Chen ,Haiqing Tang ,Yanxia Mo , Xiaojun Gu , Meizhen Chen , Weier Wu , Weimin He 1Food safety testing subsection, Ningbo entry-exit inspection and quarantine bureau technology center, Ningbo City, The Peoples Republic of China 2 Food safety testing subsection, Ningbo entry-exit inspection and quarantine bureau technology center, Ningbo City, The Peoples Republic of China 1 2 Email: yinjy@ , tanghaiqing@ Received ********* 2013. Abstract: In this study, a LC-ESI （+ ）MS/MS methodology is developed for the residue determination of methylene blue(MB). The sample was extracted by the acetonitrile and operating with a neutral alumina column solid-phase extraction column, elution after collection evaporate to dryness residue with constant volume liquid dissolve and over 0.45µm including membrane filtration, for liquid chromatography - tandem mass spectrometry determination of sample solution.Samples were detected by a gradient elution flowing with a ESI negative mode detector at MRM: m/z 285.1/269.1 ；285.1/241.0.In the line of quality assurance, When fortified with methylene blue the sample ，the stated LOQ of methylene blue residues in the negative sample was at the level of 0. 1µg/kg.The response for methylene blue was linear in the range of 0.5～50.0 μg/L,the correlation coefficient is excellent 0.999. The average recovery range was 87.6% ~ 111.2%, the coefficient of variation(CV) was 4.0% ~ 10.2%. Keywords: