Validation of capillary electrophoresis – mass spectrometry methods for the analysis of a pharmaceutical formulation

Abstract

The coupling of capillary electrophoresis (CE) to mass spectrometry (MS) with an electrospray ionization (ESI) technique is generally performed for qualitative applications, and only few quantitative results have been reported. This paper investigates the validation of a CE-ESI-MS method for the analysis of a pharmaceutical formulation containing lidocaine. Some important ESI criteria are discussed including sheath-liquid composition, nebulizing gas pressure and position of the CE capillary outlet. After optimization of these parameters, an intermediate precision of about 5% was achieved. The latter, as well as efficiency and resolution, were compared to those achieved with UV detection. Besides, a multiple injection procedure was developed to reduce analysis time per sample and was successfully applied to both UV and MS detectors. The validation results achieved by multiple injections were identical to those obtained with classical injection, but afforded a gain of time by a factor of 2.5.

Coupling CE with atmospheric pressure photoionization MS for pharmaceutical basic compounds: Optimization of operating parameters

“…In agreement with previous CE-ESI/MS experiments [52], starting conditions consisted of an i-PrOHwater (50:50 v/v) mixture containing formic acid (0.5% v/v). The addition of a dopant (toluene or acetone, from 0 to 5% v/v), the percentage of i-PrOH in water (0-100% v/v) and the proportion of formic acid (0-5% v/v) in the sheath liquid were systematically studied.…”

“…ESI capillary voltage was set at 14500 V. Nebulizing pressure and drying gas flow rate (DryF) were set at 4 psi and 4 L/min, respectively. Drying gas temperature (DryT) was set at 2507C and fragmentor voltage at 70 V. These values were selected according to Geiser et al [52].…”

“…Therefore, the latter needs to be carefully adjusted to supply an electric current created by ions reaching the entrance of the MS (CapCur) between 55 and 78 nA and an electric current produced by ions striking the end plate (ChamCur) of about 80-160 nA [52]. In CE-APPI/MS, the capillary was initially placed into the nebulizer in a similar position (about 1 mm out of the needle) [52]. The latter was labeled as position "0".…”

Densitometry, video-scanning and capillary electrophoresis for determination of valsartan and amlodipine in a combined dosage form: A comparative study

“…Meanwhile, CE is more and more frequently applied as a highly effective analytical procedure in typical pharmaceutical analysis. It has many advantages in comparison with some existing methodologies, such as lower costs and higher separation efficiency [11,12].…”

Separation window dependent multiple injection (SWDMI) for large scale analysis of therapeutic antibody N -glycans

“…The authors optimized the length of the electrolyte zone for 2x longer that of the sample zone for better resolution. Another multiple injection procedure was developed by the same authors to reduce the analysis time per sample and was successfully applied to both UV and MS detection [5]. In order to reduce analysis time, multiple injections were performed by alternatively injecting one sample zone and one BGE zone into the capillary.…”