Abstract
A simple, specific, accurate, and stability-indicating method was developed and validated for the quantitative determination of menadione sodium bisulfite in the injectable solution formulation. The method is based on zwitterionic hydrophilic interaction liquid chromatography (ZIC-HILIC) coupled with a photodiode array detector. The desired separation was achieved on the ZIC-HILIC column (250 mm × 4.6 mm, 5 μm) at 25°C temperature. The optimized mobile phase consisted of an isocratic solvent mixture of 200mM ammonium acetate (NH4AC) solution and acetonitrile (ACN) (20:80; v/v) pH-adjusted to 5.7 by glacial acetic acid. The mobile phase was fixed at 0.5 ml/min and the analytes were monitored at 261 nm using a photodiode array detector. The effects of the chromatographic conditions on the peak retention, peak USP tailing factor, and column efficiency were systematically optimized. Forced degradation experiments were carried out by exposing menadione sodium bisulfite standard and the injectable solution formulation to thermal, photolytic, oxidative, and acid-base hydrolytic stress conditions. The degradation products were well-resolved from the main peak and the excipients, thus proving that the method is a reliable, stability-indicating tool. The method was validated as per ICH and USP guidelines (USP34/NF29) and found to be adequate for the routine quantitative estimation of menadione sodium bisulfite in commercially available menadione sodium bisulfite injectable solution dosage forms.
Highlights
Menadione sodium bisulfite injectable solution is a veterinary drug which comprises vitamin K3 in the form of menadione sodium bisulfite (MSB) as the active ingredient and a mixture of inactive excipients
The MSB peak always eluted near to the void peak even when the concentration of ACN was reduced to 2.0%
Since utilizing the ion-pairing mode usually shortens the lifetime of the column as well as being an expensive reagent, this prompted us to try hydrophilic interaction liquid chromatography (HILIC) technology
Summary
Menadione sodium bisulfite injectable solution is a veterinary drug which comprises vitamin K3 in the form of menadione sodium bisulfite (MSB) as the active ingredient and a mixture of inactive excipients. There are few analytical HPLC methods that describe the HPLC analysis of vitamin K3 individually Some of these methods utilized reversed-phase ion-pairing with UV detection [2], dual-electrode amperometry [3], fluorescence [4, 5], and electrochemical detection [6]. The official BP and USP methods for MSB analysis rely on the titration of menadione as an active ingredient [8, 9]. Another USP method analyzed for menadione in the injection formulation [10]. The method is time consuming, labor intensive, and utilizes expensive and environmentally hazardous solvents
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