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

Abstract

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 time-scale 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.

Simultaneous determination of atorvastatin, amlodipine, ramipril and benazepril in human plasma by LC‐MS/MS and its application to a human pharmacokinetic study

“…The compound optimized mass parameters, DP, CE and CXP, are presented in Table 1 The most sensitive mass transition was from m/z 267.1 to 226.1, which led to the production of the product ion (data not shown). As the earlier publications have discussed extensively the fragmentation pattern of ATO (Nirogi et al, 2006), AML (Massaroti et al, 2005), RAM (Yuan et al, 2008), BEN (Vonaparti et al, 2006) and IS (nevirapine, Chi et al, 2003), we are not presenting the data pertaining to this. …”

Current Analytical Methods For Amlodipine And Its Formulations: A Review

“…the method was very raped as retention time was 1.9 for amlodipine and 3 min for nimodipine. The method was validated and all the results were satisfactory [23]. Shimooka and co-authors developed RP-HPLC method to determine amlodipine besylate in human serum using amperometric detector.…”

Determination and pharmacokinetic study of amlodipine in human plasma by ultra performance liquid chromatography–electrospray ionization mass spectrometry

“…[6,7]. Several HPLC procedures have been also reported for the analysis of amlodipine based on MS-MS detection using tandem mass spectrometry [8,9]. These reported methods are sensitive, having low quantification limits.…”