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建立了测定水产品中MS-222残留的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品经甲醇和乙腈的混合液提取,再经二氯甲烷萃取后氮气吹干,用流动相溶解,经高效液相色谱分离,以串联质谱在多反应监测模式(MRM)下进行定性与定量分析。结果表明,在1.00、10.00和50.00μg/kg添加水平下,回收率81.2%~99.5%,相对标准偏差为2.14%~4.83%(n=6)。本方法对MS-222的定量限为1.0μg/kg。该方法前处理过程简便,容易操作,灵敏度和重现性良好,结果准确。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method for the determination of MS-222 in aquatic products was established. The sample was extracted with a mixture of methanol and acetonitrile. After extraction with dichloromethane, the nitrogen was evaporated to dryness, dissolved in mobile phase and separated by high performance liquid chromatography (HPLC). Qualitative and quantitative analyzes were performed by tandem mass spectrometry in multiple reaction monitoring mode (MRM) . The results showed that the recoveries ranged from 81.2% to 99.5% with relative standard deviations of 2.14% -4.83% (n = 6) at 1.00, 10.00 and 50.00 μg / kg. The limit of quantitation of this method to MS-222 was 1.0 μg / kg. The pretreatment process of the method is simple, easy to operate, good in sensitivity and reproducibility, and accurate in result.