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    蒸发辅助-悬浮固化-分散液液微萃取-高效液相色谱法测定食用菌中3种三唑类杀菌剂的残留量

    Determination of Residues of 3 Triazole Bactericides in Edible Fungi by High Performance Liquid Chromatography Based on Evaporation-Assisted Dispersive Liquid-Liquid Microextraction with Suspension Solidification

    • 摘要: 提出了一种基于蒸发辅助和悬浮固化的分散液液微萃取结合高效液相色谱法测定食用菌中腈菌唑、联苯三唑醇、丙环唑等3种三唑类杀菌剂残留量的方法。将1.0 g食用菌样品切碎后放入10 mL离心管中,加入2 mL乙腈离心提取,取1 mL上清液和4 mL水置于10 mL离心管中,依次加入160 μL十一酸(萃取剂,密度低于水)、150 μL三氯甲烷(挥发性溶剂,密度高于水)和0.3 g氯化钠,于85 ℃加热8 min,十一酸在常温下固化后漂浮在样品溶液顶部,将上层固化物取出,加入250 μL甲醇,溶解,过0.22 μm有机滤膜。以C18色谱柱为固定相,3种三唑类杀菌剂经体积比7∶3的乙腈-水混合溶液洗脱后分离,用附二极管阵列检测器的高效液相色谱仪进行检测,以香菇、杏鲍菇、木耳、银耳、海鲜菇和金针菇6种食用菌为基质绘制工作曲线。结果表明:3种三唑类杀菌剂工作曲线的线性范围为14~1 000 μg·kg-1,检出限为4.0~5.7 μg·kg-1;对空白样品进行加标回收试验,3种三唑类杀菌剂的加标回收率为72.3%~99.4%,测定值的相对标准偏差(n=6)均小于5.5%。

       

      Abstract: A method for the determination of residues of 3 triazole bactericides, including myclobutanil, bitertanol and propiconazole, in edible fungi by high performance liquid chromatography based on evaporation-assisted dispersive liquid-liquid microextraction with suspension solidification was proposed. The edible fungus sample (1.0 g) was chopped and put into a 10 mL-centrifuge tube, and 2 mL of acetonitrile was added for extraction by centrifugation. The supernatant (1 mL) and 4 mL of water were added into a 10 mL-centrifuge tube, and 160 μL of undecanoic acid (as extraction agent, with density lower than that of water), 150 μL of trichloromethane (as volatile solvent, with density higher than that of water) and 0.30 g of sodium chloride were added successively. Then the mixed solution was heated at 85 ℃ for 8 min, and undecanoic acid was solidified at room temperature and floated on the top of the sample solution. The upper solidified substance was taken out and dissolved in 250 μL of methanol, and the solution obtained was passed through 0.22 μm organic filter membrane. The C18 column was used as stationary phase, and 3 triazole bactericides were separated after elution with the mixed solution composed of acetonitrile and water at volume ratio of 7∶3 and determined by high performance liquid chromatograph with diode array detector. The 6 edible fungi, including Lentinus edodes, Pleurotus eryngii, Auricularia auricula, Tremella fuciformis, Hypsizygus marmoreus and Flammulina velutiper, were used as matrixes to draw working curves. It was shown that the linear ranges of 3 triazole bactericides were 14-1 000 μg·kg-1, with detection limits in the range of 4.0-5.7 μg·kg-1. Test for recovery was made on the blank samples by standard addition method, giving results in the range of 72.3%-99.4%, with RSDs (n=6) of the determined values less than 5.5%.

       

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