title: 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.
authors.affiliation: Dept. of Hygiene Analytical Chemistry, School of Public Health, Shandong Univ., 44 Wenhua West Road, Box 104, Jinan 250012, China.
authors.forename: Guanmin
authors.initials: G
authors.lastname: Su
authors.forename: Xifeng
authors.initials: X
authors.lastname: Wang
authors.forename: Defeng
authors.initials: D
authors.lastname: Chi
authors.forename: Lin
authors.initials: L
authors.lastname: Li
authors.forename: Lihua
authors.initials: L
authors.lastname: Shao
mesh_terms: D009327:4-Chloro-7-nitrobenzofurazan / Q000031:analogs & derivatives / Q000378:metabolism; D000097:Acetonitriles / Q000378:metabolism; D002138:Calibration; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D058870:Food, Organic / Q000032:analysis*; D005944:Glucosamine / Q000302:isolation & purification*; D010710:Phosphates / Q000378:metabolism; D017680:Potassium Compounds / Q000378:metabolism; D015203:Reproducibility of Results; D059629:Signal-To-Noise Ratio; D013696:Temperature; D014269:Trifluoroacetic Acid / Q000378:metabolism
chemical_list: D000097:Acetonitriles; D010710:Phosphates; D017680:Potassium Compounds; C032930:7-fluoro-4-nitrobenzo-2-oxa-1,3-diazole; C013216:potassium phosphate; D014269:Trifluoroacetic Acid; D009327:4-Chloro-7-nitrobenzofurazan; D005944:Glucosamine; C032159:acetonitrile