固相分散萃取与气相色谱-负化学离子源质谱联用法测定食品中三唑醇的残留量

Determination of triadimenol residue in foods with dispersive solid phase extraction cleanup by gas chromatography-negative chemical ionization mass spectrometry

建立了食品中三唑醇残留量的固相分散萃取-气相色谱-负化学离子源质谱联用检测方法。样品中三唑醇残留物由正己烷饱和的乙腈（含1％冰醋酸）提取，加入无水硫酸镁与无水醋酸钠振荡促使提取液分层后进行固相分散萃取净化，用气相色谱-负化学离子源质谱法进行测定与确证，外标法定量。方法具有良好的选择性和抗干扰能力，其检出限和定量限分别为0．001mg／kg和0．003mg/kg；线性范围为0．050～0．750mg／L，相关系数为0．9947；在0．005，0．010，0．020mg／kg共3个添加水平下的平均回收率为70％～110％，相对标准偏差不大于12．0％。该方法适合于多种食品中三唑醇残留量的确证分析。

A confirmatory method is presented for the determination of triadimenol residue in foods by dispersive solid phase extraction-gas chromatography-negative chemical ionization mass spectrometry （SPE-GC-NCI/MS）. Triadimenol residue was extracted from different food samples, such as snow pea, carrot, orange, bean, spinach, oolong tea, rice, beef, longsnout catfish, royel jelly, red swamp crayfish, bee honey etc with acetonitrile containing 1% acetic acid and simultaneous liquid-liquid partitioning formed by adding anhydrous magnesium sulfate plus sodium acetate, followed by a simple clean-up step known by dispersive solid-phase extraction. The aliquot was determined and confirmed by gas chromatography-negative chemical ionization mass spectrometry using external standard method. The average recoveries at the three spiked levels （0. 005, 0. 010 and 0. 020 mg/kg） in different samples ranged from 70% to 110%, and the relative standard deviations were lower than 12.0%. The linearity of detection ranged from 0. 050 to 0. 750 mg/L. The detection limit of the method was 0. 001 mg/kg and the limit of quantification was 0. 003 mg/kg. The method is selective with no interference and suitable for confirmatory of triadimenol residue in 12 categories of foods.