A new method for sensitive and rapid indirect electrochemiluminescence(IECL)detection of norepinephrine(NE),synephrine,and isoproterenol with capillary electrophoresis(CE)was developed.IECL detection is based on their...A new method for sensitive and rapid indirect electrochemiluminescence(IECL)detection of norepinephrine(NE),synephrine,and isoproterenol with capillary electrophoresis(CE)was developed.IECL detection is based on their quenching effects on Ru(bpy)2+3/tripropylamine(TPA)system.Under the optimum conditions,the detection limits(S/N=3)were 2.6×10-8 mol/L for NE,6.6×10-9 mol/L for synephrine,and 8.4×10-8 mol/L for isoproterenol.The RSD of migration time and peak area were less than 1.3% and 4.4%,respectively.The proposed method was successfully applied to the analysis of NE in the urine samples of 10 healthy people and 10 diabetic nephropathy patients.The results indicate that the content of NE in diabetic nephropathy patients is much higher than that in healthy people.展开更多
A new approach for the determination of methylephedrine hydrochloride(ME),thebaine,codeine phosphate(CP),and acetylcodeine(AC) was established by CE-ECL with ionic liquid(1-butyl-3-methylimidazolium tetrafluoroborate,...A new approach for the determination of methylephedrine hydrochloride(ME),thebaine,codeine phosphate(CP),and acetylcodeine(AC) was established by CE-ECL with ionic liquid(1-butyl-3-methylimidazolium tetrafluoroborate,BMIMBF4). The conditions for the CE separation,ECL detection and the effect of ionic liquid(IL) were systematically investigated. Under the optimal conditions,the four analytes were well separated within 8 min using BMIMBF4 as additive in the electrophoretic buffer. The concentration detection limits of ME,thebaine,CP,and AC were 2.1×10-8,1.4×10-7,6.3×10-8,and 3.6×10-8 mol/L(S/N=3),respectively. The limits of quantitation(LOQ,S/N=10) in real human urine samples were 7.6×10-7 mol/L for ME,3.6 ×10-6 mol/L for thebaine,6.5×10-7 mol/L for CP,and 4.6×10-7 mol/L for AC,respectively. The recoveries of four alkaloids at different levels in human urine samples were between 90.0% and 103.5%. The developed method was successfully applied to the determination of four drug alkaloids in human urine samples.展开更多
The separation and determination of captopril in human serum and urine samples by means of high performance liquid chromatography(HPLC) with on-line electrogenerated Mn(Ⅲ) chemiluminescence detection was carried out....The separation and determination of captopril in human serum and urine samples by means of high performance liquid chromatography(HPLC) with on-line electrogenerated Mn(Ⅲ) chemiluminescence detection was carried out. The method was based on the direct chemiluminescence reaction between captopril and Mn(Ⅲ), which was on-line electrogenerated by constant current electrolysis. The chromatographic separation was performed on a nucleosil RP-C18(250 mm×4.6mm i.d., 5 μm) column with an isocratic mobile phase consisting of acetonitrile-1% aqueous acetic acid(volume ratio 6∶4) at a flow-rate of 1.2 mL/min. The temperature was 25 ℃. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. Under the optimal conditions, the linear range and detection limit for captopril are 5—800 ng/mL and 0.9 ng/mL, respectively. The relative standard derivation for 10.0 ng/mL captopril is 2.2%(n=11). The average recoveries for captopril in human serum and urine samples ranged from 94.8% to 103.2%, and the relative standard deviations of the quantitative results are below 3.4%. The proposed method had been applied to the determination of captopril in human serum and urine samples.展开更多
文摘A new method for sensitive and rapid indirect electrochemiluminescence(IECL)detection of norepinephrine(NE),synephrine,and isoproterenol with capillary electrophoresis(CE)was developed.IECL detection is based on their quenching effects on Ru(bpy)2+3/tripropylamine(TPA)system.Under the optimum conditions,the detection limits(S/N=3)were 2.6×10-8 mol/L for NE,6.6×10-9 mol/L for synephrine,and 8.4×10-8 mol/L for isoproterenol.The RSD of migration time and peak area were less than 1.3% and 4.4%,respectively.The proposed method was successfully applied to the analysis of NE in the urine samples of 10 healthy people and 10 diabetic nephropathy patients.The results indicate that the content of NE in diabetic nephropathy patients is much higher than that in healthy people.
文摘A new approach for the determination of methylephedrine hydrochloride(ME),thebaine,codeine phosphate(CP),and acetylcodeine(AC) was established by CE-ECL with ionic liquid(1-butyl-3-methylimidazolium tetrafluoroborate,BMIMBF4). The conditions for the CE separation,ECL detection and the effect of ionic liquid(IL) were systematically investigated. Under the optimal conditions,the four analytes were well separated within 8 min using BMIMBF4 as additive in the electrophoretic buffer. The concentration detection limits of ME,thebaine,CP,and AC were 2.1×10-8,1.4×10-7,6.3×10-8,and 3.6×10-8 mol/L(S/N=3),respectively. The limits of quantitation(LOQ,S/N=10) in real human urine samples were 7.6×10-7 mol/L for ME,3.6 ×10-6 mol/L for thebaine,6.5×10-7 mol/L for CP,and 4.6×10-7 mol/L for AC,respectively. The recoveries of four alkaloids at different levels in human urine samples were between 90.0% and 103.5%. The developed method was successfully applied to the determination of four drug alkaloids in human urine samples.
文摘The separation and determination of captopril in human serum and urine samples by means of high performance liquid chromatography(HPLC) with on-line electrogenerated Mn(Ⅲ) chemiluminescence detection was carried out. The method was based on the direct chemiluminescence reaction between captopril and Mn(Ⅲ), which was on-line electrogenerated by constant current electrolysis. The chromatographic separation was performed on a nucleosil RP-C18(250 mm×4.6mm i.d., 5 μm) column with an isocratic mobile phase consisting of acetonitrile-1% aqueous acetic acid(volume ratio 6∶4) at a flow-rate of 1.2 mL/min. The temperature was 25 ℃. The effects of several parameters on the HPLC resolution and CL emission were studied systematically. Under the optimal conditions, the linear range and detection limit for captopril are 5—800 ng/mL and 0.9 ng/mL, respectively. The relative standard derivation for 10.0 ng/mL captopril is 2.2%(n=11). The average recoveries for captopril in human serum and urine samples ranged from 94.8% to 103.2%, and the relative standard deviations of the quantitative results are below 3.4%. The proposed method had been applied to the determination of captopril in human serum and urine samples.
