Improved Determination of d‐Glucosamine Hydrochloride in Health Foods by HPLC Using 7‐Fluoro‐4‐Nitrobenzo‐2‐Oxa‐l,3‐Diazole as a Derivative

Abstract

This article presents an improved method to detect D-glucosamine hydrochloride in health foods. A simple precolumn derivatization procedure with 7-flouro-4-nitrobenzo-2-oxa-1,3-diazole (NBD-F) reagent was employed. The separation of the derivatized D-glucosamine hydrochloride (NBD-D-glucosamine hydrochloride) was performed using a mobile phase consisting of acetonitrile, potassium dihydrogen phosphate (0.01 mol/L), and trifluoroacetic acid (350:649.74:0.26, volume ratio) at a flow rate of 1.0 mL/min with the column temperature 35 °C. Under the optimum chromatographic conditions, the peak area of NBD-D-glucosamine hydrochloride compared with its absolute value of the peak area of NBD-D-glucosamine hydrochloride in a standard solution concentration range from 1.0 to 500.0 mg/L showed a good linear calibration (R = 0.9999). Recoveries, at spiked concentrations of 10.0, 40.0, and 500.0 mg/L, varied between 97.2% and 102.6% with relative standard deviations ranging from 0.4% to 1.5%. The present method provides sufficient sensitivity as reflected by the values of limit of detection (LOD) and limit of quantification (LOQ). LOD was determined from the signal-to-noise ratios (S/N) of NBD-D-glucosamine hydrochloride peak of at least 3 in the recovery test at 0.02 mg/L, and the estimated LOQ was 0.06 mg/L (S/N = 10). The proposed method was successfully applicable to detect D-glucosamine hydrochloride in health foods and drugs containing a variety of complex materials.

Determination of glucosamine and monitoring of its mutarotation by hydrophilic interaction liquid chromatography with evaporative light scattering detector

“…A common liquid chromatographic mode is RPHPLC on a C 8 or C 18 column with various detectors. Way et al have suggested a refractive detector (Way, Gibson, & Breite, 2000), but typically (after derivatization) either UV detection (Lopez-Cervantes, Sanchez-Machado, & Delgado-Rosas, 2007;Su, Wang, Chi, Li, & Shao, 2011;Kosman, Karlina, Pozharitskaya, Shikov, & Makarov, 2017) or more sensitive fluorescence detection has been applied Nemati, Valizadeh, Ansarin, & Ghaderi, 2007;Ibrahim & Jamali, 2010). Recently, also MS detection has been reported for a pharmacokinetic study (Song, Hang, Wang, Yang, & Wen, 2012).…”