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

作　　者：周莉[1] 王新全[1] 徐浩[1] 王祥云[1] 刘芯成[1] 刘之炜[1] 刘秋菊[1] 章虎[1] 

机构地区：[1]浙江省农业科学院农产品质量标准研究所,农业部农药残留检测重点实验室,杭州310021

出　　处：《理化检验（化学分册）》2011年第12期1398-1401,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家高技术研究发展计划项目(2011AA100806)

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3mL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5mL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。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.

关 键 词：液相色谱-串联质谱法 叶菜类蔬菜 基质效应 农药 

分 类 号：O657.63[理学—分析化学]