Stability‐indicating assay of sodium cromoglicate in ophthalmic solution using mixed‐mode hydrophilic interaction chromatography

Abstract

A hydrophilic interaction chromatographic (HILIC) procedure for the quantification of Sodium Cromoglicate (SCG) in ophthalmic solution is developed. Mobile phase consists of ACN and buffer, 86:14 v/v. Atlantis HILIC-Si column, 25 cm x 4.6 mm, is used as stationary phase. Detection is carried out using a variable wavelength UV-Vis detector at 326 nm. Linearity range and percent recoveries for SCG were 50-400 mug/mL and 100.44%, respectively. The SCG HILIC-UV assay was validated according to the International Conference on Harmonization guidelines. The method separates two impurities and degradation products resulting from stress environment. Influence of organic solvent, ionic strength and mobile phase pH on the retention of SCG is studied. The paper provides optimization of polar anionic solute (SCG) on unmodified silica by HILIC. Proposed method can be used as a stability-indicating assay for SGC and can be proved to be beneficial in ESI-MS for enhanced sensitivity.

HILIC methods in pharmaceutical analysis

“…After optimization of the HILIC assays, most were validated, occasionally according to a guideline. The United States Pharmacopeia 88 was followed in 51, the International Conference on Harmonisation of Technical Requirements for the Registration of Pharmaceuticals for Human Use 89 in 27, 35, 57, 63, 69, 71, the US Food and Drug Administration (FDA) 90 in 24–26, 28, 34, 39, 40, 56, 58, 62, 67, 80, and the guideline of the AIDS Clinical Trials Group 91, which is based on the FDA guideline in 43. No reference to a guideline was made in 21, 22, 29, 30, 32, 33, 36–38, 42, 45–50, 52, 59–61, 66, 70, 72, 79, 81.…”

“…The examined validation topics were linearity of the calibration curve 21, 22, 24–30, 32–40, 42, 43, 45–52, 56–63, 66, 67, 69–72, 79–81, limit of detection 27, 28, 32, 33, 35, 36, 38, 40, 45, 51, 58, 67, 69, 72, (lower) limit of quantification 21, 22, 24–28, 30, 32–37, 39, 42, 43, 45–52, 56–58, 60–63, 66, 67, 69, 70, 79, 80, precision estimates (repeatability and/or time‐different intermediate precision) 21, 22, 24–30, 32–40, 42, 43, 45–52, 56–63, 66, 67, 69, 70, 72, 79–81, accuracy, trueness, and/or recovery 21, 22, 24–30, 32–40, 42, 43, 45–52, 56–63, 66, 67...…”

“…A large diversity of pharmaceutical compounds, belonging to different therapeutical classes, has been analyzed in HILIC mode using bare‐silica as SP 21–52. Both non‐biological 27, 31, 35, 36, 38, 41, 44, 51 and biological 21–26, 28–30, 32–34, 37, 39, 40, 42, 43, 45–50, 52 assays are described. The finally reported experimental conditions are presented in Table 1.…”

“…HILIC was used to analyze active pharmaceutical ingredients (APIs) in formulations in 27, 35, 51. In cough–cold formulations, the sympathomimetic decongestivum pseudoephedrine.HCl, the antihistaminicum diphenhydramine.HCl, and the antitussivum dextromethorphan.HBr were determined simultaneously 27.…”

“…The HILIC method (Supelcosil SIL) resulted in baseline‐separated peaks. In an ophthalmic solution, the antiallergic agent sodium cromoglicate was analyzed 35. In tablet formulations, the antidiabetic drug metformin and its related compound 1‐cyanoguanidine were determined 51.…”