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固相萃取-液质联用法测定食品中两种苯氧乙酸类除草剂含量
Determination of two kinds of phenoxy acid herbicides in foods by solid phase extraction and high performance liquid chromatography-mass spectrum
【摘要】 建立了固相萃取-液质联用法测定食品中2,4-二氯苯氧乙酸(2,4-D)和2-甲-4-氯苯氧乙酸(MCPA)含量的方法。样品经0.01 mol/L氢氧化钠碱液提取后,用甲酸溶液调至酸性(pH=3.0),以Oasis HLB柱净化富集,在HPLC-MS(SIR)模式下进行定性定量分析。结果表明,2,4-D和MCPA溶液在0.005~0.32μg/mL内呈良好的线性关系,相关系数r分别为0.999 3和0.999 6,检出限(S/N=3)分别为1.35,1.31μg/L,富集倍数为49和51,加标回收率为78.75%~103.75%。本法操作简便、结果准确、重复性好,是测定食品中残留2,4-D和MCPA含量的有效方法。
【Abstract】 A method for the determination of 2,4-D and MCPA in foods was established by solid phase extraction and HPLC-MS.The samples were extracted by 0.01 mol/L sodium hydroxide solution firstly,adjusted to pH=3.0 with formic acid,then purified and enriched by Oasis HLB solid phase extraction column.Qualitative and quantitative analysis were carried out under the SIR mode after the chromatography separation.The experiment results showed good linear relationships were obtained in the concentrations from 0.005 ~ 0.32 μg/mL with the correlation coefficient 0.999 3 and 0.999 6.The detection limits were 1.35,1.31 μg/L(S/N=3).The enrichment factors were 49 and 51.The recoveries were in the range from 78.75% to 103.75%.This method was easy to operate with precise result ahd good repetition,which can be successfully applied to the determination of 2,4-D and MCPA in other foods.
- 【文献出处】 应用化工 ,Applied Chemical Industry , 编辑部邮箱 ,2011年08期
- 【分类号】R155.5
- 【被引频次】4
- 【下载频次】184