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目的采用液相色谱-串联质谱法测定市售生牡蛎中孔雀石绿、隐色孔雀石绿、结晶紫与隐色结晶紫残留。方法样品溶液加入氘代混合内标,酸性氧化铝固相萃取小柱净化后过WAX小柱分离,用乙腈对WAX小柱进行洗脱后氮气吹干,残余物溶于50%乙腈水溶液后上液相色谱-串联质谱仪测定,梯度流动相为乙腈:5mmol/L乙酸铵溶液。结果各分子在0.5～10μg/kg浓度范围线性关系良好,平均回收率68.54%～89.63%,质谱仪定量限在0.0313～0.0621μg/kg。结论该方法灵敏准确,专属性强,干扰少,重现性佳,对检测贝类水产品中的三苯甲烷类染料残留极具参考价值。
Objective To determine the residual malachite green, leucomalachite green, crystal violet and leuco crystal violet in commercial raw oysters by liquid chromatography-tandem mass spectrometry. Methods The sample solution was deuterated and mixed with an internal standard. The acidic alumina solid phase extraction cartridge was purified and then separated on a WAX cartridge. The WAX cartridge was eluted with acetonitrile and then blown dry. The residue was dissolved in 50% acetonitrile in water Liquid chromatography - tandem mass spectrometry, gradient mobile phase acetonitrile: 5mmol / L ammonium acetate solution. Results The linearity of each molecule ranged from 0.5μg / kg to 10μg / kg. The average recovery was 68.54% ~ 89.63%. The limit of quantification was 0.0313 ~ 0.0621μg / kg. Conclusion The method is sensitive, accurate, specific, less interference and reproducible. It is very useful for the determination of triphenylmethane dyes in shellfish aquatic products.