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    液相色谱-串联质谱法测定叶菜类蔬菜中16种农药的基质效应研究

    On the Matrix Effects in the LC-MS/MS Determination of 16 Pesticides in Leaf Vegetables

    • 摘要: 应用液相色谱-串联质谱法研究了6种叶菜类蔬菜中16种农药的基质效应。用乙腈提取叶菜样品中农药,过滤后的提取液与固体氢化钠充分混匀,分取部分澄清液,在减压条件下蒸至近干,再经吹氮至干,残渣溶于乙腈-甲苯(3+1)混合液3 mL中,经Envi-carb-NH2柱进行纯化。收集淋出液,先后在40 ℃减压蒸发及吹氮将溶液蒸干,用甲醇溶解残渣,甲醇-水(1+1)混合溶液定容为5 mL进行分析。分别在加入基质和不加基质的条件下制作标准工作曲线,据所得数据及两者的斜率比对测定中的基质效应作出评估。结果表明:试样溶液经Envi-carb-NH2柱纯化后,在16种农药中有12种农药测定中的基体效应得到消除,可直接用不加基质的标准工作曲线进行定量。

       

      Abstract: A study on the matrix effects in the LC-MS/MS determination of 16 pesticides in 6 kinds of leaf vagetables was reported. Sample of leaf-vegetable was extracted with acetonitrile, and filtered. The filtrate was mixed with solid NaCl and an aliquot was taken for purification by passing through the SPE microcolumn (Envi-carb-NH2 column), after evaporation to dryness and dissolution of the residue in 3 mL of CH3CN+toluene (3+1) mixture. The eluates were collected and evaporated to drycess at 40 ℃ under reduced pressure and by N2-blowing in succession. The residue was taken up with methanol and made up to 5 mL with CH3OH+H2O (1+1) mixture. Standard working curves were prepared by using standard solutions of the 16 pesticides with and without addition of sample matrixes, and the matrix effects were evaluated on the base of the experimental data and values of slope ratios obtained. It was found that by applying the SPE purification with Envi-carb-NH2 column, matrix effects were eliminated in the determination of 12 among the 16 pesticides studied, and standard working curves without addition of sample matrix were used in the determinations.

       

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