Sensitive Method for the Quantitative Determination of Ergotamine in Tablet Dosage Form by High-Performance Liquid Chromatography Using Bromocriptine as Internal Standard

Aim: To develop and validate a selective, sensitive and simple RP-HPLC method for the determination of ergotamine tartrate (ET) in pharmaceutical dosage forms.

Study Design: All variables were studied to optimize the chromatographic conditions.

Place and Duration of Study: Department of Chemistry, Faculty of Science, Aleppo University, Aleppo, Syria during seven months.

Methodology: The chromatographic separation of ET and bromocriptine mesylate (BCM, was used as internal standard) was achieved on a reversed phase BDS Hypersil C8 column (250×4.6 mm i.d., 5 mm particle size) with a mobile phase consisted of MeOH-HCOOH 0.1 M (70:30, v/v), pumped at a flow rate 1.0 mL min-1 and detected at 320 nm.

Results: The retention times were 8.30 and 10.93 min for ET and BCM, respectively. The validation of the proposed method was carried out for specificity, linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. Linearity range was 3.0-1400.0 mg mL-1 with limits of detection and quantification values of 0.18 and 0.58 μg mL-1, respectively. The precision of the method was demonstrated using intra- and inter-day assay RSD values which were less than 2.35% in all instances, while the relative percentage error was less than 1.99% (n=6). No interference from any components of pharmaceutical dosage forms or degradation products was observed.

Conclusion: The developed method was found to be selective, accurate, precise, robust and could be applied to the quantitative analysis of ET in raw material and tablets.