Isolation and Characterization of Related Impurities of Monoammonium Glycyrrhizinate and Development of RP-HPLC Method for Quality Control Study

Abstract

An HPLC method was developed for the determination of impurities of monoammonium glycyrrhizinate in bulk drugs and pharmaceutical formulations. The separation was accomplished on a Shimadzu Shim-pack C₁₈ (150 mm × 4.6 mm, 5 µm) column. The mobile phase was methanol: (0.2 M) ammonium acetate (70:30; v/v, pH = 4.5) and a UV detector set at 250 nm was used for detection. The unknown impurities were isolated by preparative HPLC and characterized by FT-IR, ESI-MS, ¹H NMR and ¹³C NMR spectral data. The proposed method was validated and successfully applied to the analysis of commercial bulk drugs and formulations, thus it supplied a simple and sensitive method to ensure the quality assurance for the manufactures and researches.

Keywords:

• Glycyrrhizin
• Isolation and characterization
• Monoammonium glycyrrhizinate
• Related impurities

Notes

The chemical shifts (δ values) are given in parts per million (ppm).

The coupling constant (J values) are reported in hertz (Hz).

S, singlet; d, doublet; t, triplet; q, quartet; br, broad; m, multiplet; o, overlapped.

A: peak area; C: concentration.