Development and validation of a selective and robust LC-MS/MS method for quantifying amlodipine in human plasma

被引:36
作者
Massaroti, P [1 ]
Moraes, LAB [1 ]
Marchioretto, MAM [1 ]
Cassiano, NM [1 ]
Bernasconi, G [1 ]
Calafatti, SA [1 ]
Barros, FAP [1 ]
Meurer, EC [1 ]
Pedrazzoli, J [1 ]
机构
[1] Univ Sao Francisco, Sch Med, Clin Pharmacol & Gastroenterol Unit, BR-12916900 Braganca Paulista, SP, Brazil
关键词
mass spectrometry; bioequivalence; amlodipine;
D O I
10.1007/s00216-005-3227-z
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A liquid chromatographic-tandem mass spectrometric method (LC-MS/MS) for quantifying amlodipine in human plasma was developed and validated. Sample preparation was based on liquid-liquid extraction using NaOH and a mixture of ethyl acetate/hexane (80/20; v/v). Chromatography was performed on a C-18 analytical column and the retention times were 1.9 and 3.0 min for amlodipine and nimodipine (internal standard), respectively. The ionization was optimized using ESI(+) and enhanced selectivity was achieved using tandem mass spectrometric analysis via two MRM functions, 409 -> 238 and 418 -> 343 for amlodipine and nimodipine. The calibration curve ranged from 0.2 to 20.0 ng/mL. The inter-day precision and accuracy and the relative standard deviation (RSD) were < 15%. The analyte was shown to be stable over the timescale of the whole procedure. The robustness of the method was demonstrated by the good reproducibility of the results obtained during the analysis of clinical samples.
引用
收藏
页码:1049 / 1054
页数:6
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