建立了韭菜中11种氨基甲酸酯农药残留的液相色谱串联质谱分析方法,本试验对2种前处理方法(农业部761—2008前处理法、QuEChERS前处理法)进行考察,线性范围在0.5~50.0 ng/mL,线性相关系数0.991~0.999。使用Agilent Bond Elut QuEChERS试...建立了韭菜中11种氨基甲酸酯农药残留的液相色谱串联质谱分析方法,本试验对2种前处理方法(农业部761—2008前处理法、QuEChERS前处理法)进行考察,线性范围在0.5~50.0 ng/mL,线性相关系数0.991~0.999。使用Agilent Bond Elut QuEChERS试剂盒以及NY/T761-2008的前处理方法分别对韭菜进行前处理,QuEChERS方法、农业部761前处理方法的回收率分别为71.23%~100.37%、70.49%~108.32%。结果表明,QuEChERS方法具有操作简便快速、准确率高、重复性好等优点。展开更多
This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was us...This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.展开更多
文摘建立了韭菜中11种氨基甲酸酯农药残留的液相色谱串联质谱分析方法,本试验对2种前处理方法(农业部761—2008前处理法、QuEChERS前处理法)进行考察,线性范围在0.5~50.0 ng/mL,线性相关系数0.991~0.999。使用Agilent Bond Elut QuEChERS试剂盒以及NY/T761-2008的前处理方法分别对韭菜进行前处理,QuEChERS方法、农业部761前处理方法的回收率分别为71.23%~100.37%、70.49%~108.32%。结果表明,QuEChERS方法具有操作简便快速、准确率高、重复性好等优点。
文摘This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.
