Shen Weijian, Lin Hong, Zhao Zengyun, Ding Tao, Xu Jinzhong, Shen Chongyu
Food Laboratory of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China.
Se Pu. 2008 Jul;26(4):515-8.
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.
建立了一种采用分散固相萃取-气相色谱-负化学电离质谱法（SPE-GC-NCI/MS）测定食品中三唑醇残留量的确证方法。用含1%乙酸的乙腈从不同食品样品（如雪豌豆、胡萝卜、橙子、豆类、菠菜、乌龙茶、大米、牛肉、长吻鮠、蜂王浆、克氏原螯虾、蜂蜜等）中提取三唑醇残留，加入无水硫酸镁和乙酸钠进行液液分配，随后通过分散固相萃取进行简单净化。取等分试样，采用外标法通过气相色谱-负化学电离质谱法进行测定和确证。不同样品在三个加标水平（0.005、0.010和0.020 mg/kg）下的平均回收率为70%至110%，相对标准偏差低于12.0%。检测线性范围为0.050至0.750 mg/L。该方法的检测限为0.001 mg/kg，定量限为0.003 mg/kg。该方法具有选择性，无干扰，适用于12类食品中三唑醇残留的确证。
