Quantitative HPLC Analysis of Active Pharmaceutical Ingredients in Syrup Vehicle Using Centrifugal Filter Devices and Determination of Xanthan Gum in Syrup Vehicle Using Rheometry

Abstract

Using rapid centrifugal filtration (<or= 30 min) of diluted samples, the filter membrane prevented compounds with molecular weight higher than the nominal molecular weight limit (NMWL) from transporting through the membrane, thus separating them from compounds with molecular weight smaller than NMWL, which would pass through the membrane. The purpose of this study aims to remove high molecular weight matrix (such as xanthan gum) interferences while achieving a quantitative analysis of the active pharmaceutical ingradients of interest. Two model active pharmaceutical ingredients, L-arginine and amphotericin B, were quantitatively recovered from the diluted syrup vehicle after centrifugation with the filter devices. The reproducibility [% relative standard deviation (RSD), peak area] of the filtered samples was less than 0.5%. For amphotericin B samples. The linear range was 0.28 microg/mL to 28.2 microg/mL. The limit of detection was 0.06 microg/mL. The limit of quantification was 0.28 microg/mL. The viscosity of a syrup vehicle changed linearly with the concentration of xanthan gum. A method was thus developed to determine xanthan gum in the syrup vehicle. The accuracy was within 95.0% to 105.0% at different concentration levels.

Validation of an UPLC-DAD Method for the Quantification of Phenolic Acids, Verbascoside and 6-epi-aucubin in Crescentia cujete Fruit

“…An aliquot (1 mL) of this solution was transferred into a centrifugal filter device. Centrifugation was performed at 5000 rpm for 30 min [5]. The filtrate was diluted into a 10 mL volumetric flask with water.…”

“…Samples were stored at −20 °C prior to analysis, if necessary. Centrifugal filters were selected for removing xanthan gums from the matrix of commercial samples that may be present in many syrups [5]. Xanthan gum would be extremely difficult to eliminate under normal HPLC conditions, thus affecting peak shapes, deteriorating the column efficiency, or damaging the column.…”