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Improved Determination of d ‐Glucosamine Hydrochloride in Health Foods by HPLC Using 7‐Fluoro‐4‐Nitrobenzo‐2‐Oxa‐l,3‐Diazole as a Derivative
Author(s) -
Su Guanmin,
Wang Xifeng,
Chi Defeng,
Li Lin,
Shao Lihua
Publication year - 2011
Publication title -
journal of food science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.772
H-Index - 150
eISSN - 1750-3841
pISSN - 0022-1147
DOI - 10.1111/j.1750-3841.2011.02380.x
Subject(s) - chemistry , detection limit , chromatography , glucosamine , hydrochloride , derivatization , reagent , trifluoroacetic acid , acetonitrile , high performance liquid chromatography , calibration curve , organic chemistry
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.