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
建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取...建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。展开更多
建立固相萃取-液相色谱-串联质谱法测定地下水中44种抗生素。调节样品pH值为3,加入质量浓度为0.5 g/L Na_(2)EDTA,用5 mL 0.1%甲酸-甲醇和3 mL 5%氨水-甲醇以流速为2 mL/min洗脱,动态多反应监测分析。结果表明,44种抗生素在质量浓度为0...建立固相萃取-液相色谱-串联质谱法测定地下水中44种抗生素。调节样品pH值为3,加入质量浓度为0.5 g/L Na_(2)EDTA,用5 mL 0.1%甲酸-甲醇和3 mL 5%氨水-甲醇以流速为2 mL/min洗脱,动态多反应监测分析。结果表明,44种抗生素在质量浓度为0~50μg/L时,线性相关系数大于0.990,方法检出限为0.05~0.90 ng/L,加标回收率为39.1%~143%,RSD为1.9%~14%。采用该方法测定苏北某地地下水,检出18种抗生素(质量浓度为ND~21.7 ng/L)。展开更多
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.
文摘建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。
文摘建立固相萃取-液相色谱-串联质谱法测定地下水中44种抗生素。调节样品pH值为3,加入质量浓度为0.5 g/L Na_(2)EDTA,用5 mL 0.1%甲酸-甲醇和3 mL 5%氨水-甲醇以流速为2 mL/min洗脱,动态多反应监测分析。结果表明,44种抗生素在质量浓度为0~50μg/L时,线性相关系数大于0.990,方法检出限为0.05~0.90 ng/L,加标回收率为39.1%~143%,RSD为1.9%~14%。采用该方法测定苏北某地地下水,检出18种抗生素(质量浓度为ND~21.7 ng/L)。
