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  • Development and validation of LC methods for the separation of misoprostol related substances and diastereoisomers.

Development and validation of LC methods for the separation of misoprostol related substances and diastereoisomers.

Journal of pharmaceutical and biomedical analysis (2015-04-17)
Getu Kahsay, Huiying Song, Fran Eerdekens, Yaxin Tie, Danny Hendriks, Ann Van Schepdael, Deirdre Cabooter, Erwin Adams
ABSTRACT

Misoprostol is a synthetic prostaglandin E1 analogue which is mainly used for prevention and treatment of gastric ulcers, but also for abortion due to its labour inducing effect. Misoprostol exists as a mixture of diastereoisomers (1:1) and has several related impurities owing to its instability at higher temperatures and moisture. A simple and robust reversed phase liquid chromatographic (RPLC) method is described for the separation of the related substances and a normal phase (NP) LC method for the separation of misoprostol diastereoisomers. The RPLC method was performed using an Ascentis Express C18 (150 mm × 4.6 mm, 5 μm) column kept at 35 °C. The mobile phase was a gradient mixture of mobile phase A (ACN-H2O-MeOH, 28:69:3 v/v/v) and mobile phase B (ACN-H2O-MeOH, 47:50:3 v/v/v) eluted at a flow rate of 1.5 mL/min. UV detection was performed at 200 nm. The NPLC method was undertaken by using an XBridge bare silica (150 mm × 2.1 mm, 3.5 μm) column at 35 °C. The mobile phase contained 1-propanol-heptane-TFA (4:96:0.1%, v/v/v), pumped at a flow rate of 0.5 mL/min. UV detection was performed at 205 nm. This LC method can properly separate the two diastereoisomers (Rs > 2) within an analysis time of less than 20 min. Both methods were validated according to the ICH guidelines. Furthermore, these new LC methods have been successfully applied for purity control and diastereoisomers ratio determination of misoprostol bulk drug, tablets and dispersion.

MATERIALS
Product Number
Brand
Product Description

Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 4.6 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 2 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 25 cm × 3 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 3 cm × 4.6 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 7.5 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 5 cm × 4.6 mm
Supelco
Ascentis® Express C18, 2 μm Guard Cartridge, 2 μm particle size, L × I.D. 5 mm × 2.1 mm, pkg of 3 ea
Supelco
Ascentis® Express C18, 5 μm HPLC Column, 5 μm particle size, L × I.D. 15 cm × 2.1 mm
Sigma-Aldrich
Ethanol Fixative 80% v/v, suitable for fixing solution (blood films)
Supelco
Ethanol standards 10% (v/v), 10 % (v/v) in H2O, analytical standard
Supelco
Ascentis® Si HPLC Column, 3 μm particle size, L × I.D. 3 cm × 2.1 mm
Supelco
Ascentis® Si HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
Ascentis® Si HPLC Column, 5 μm particle size, L × I.D. 25 cm × 2.1 mm
Supelco
Ascentis® Si HPLC Column, 5 μm particle size, L × I.D. 25 cm × 10 mm
Supelco
Ascentis® Si HPLC Column, 3 μm particle size, L × I.D. 15 cm × 2.1 mm
Supelco
Ascentis® Si HPLC Column, 5 μm particle size, L × I.D. 10 cm × 2.1 mm
Supelco
Ascentis® Si HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
Ascentis® Si HPLC Column, 5 μm particle size, L × I.D. 25 cm × 21.2 mm