Determination of Glucosamine in Raw Materials and Dietary Supplements Containing Glucosamine Sulfate and/or Glucosamine Hydrochloride by High-Performance Liquid Chromatography with FMOC-Su Derivatization: Collaborative Study

Abstract

A collaborative study was conducted for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by high-performance liquid chromatography (HPLC) with N-(9-fluorenyl-methoxycarbonyloxy) succinimide (FMOC-Su) derivatization. Thirteen blind materials, one pair of which were duplicates, were tested by 12 collaborating laboratories. The test samples consisted of various commercial products, including tablets, capsules, drink mix, and liquids as well as raw materials, blanks, and those for spike recovery analyses. The tests with blank products and products spiked with glucosamine showed good specificity of the method. The average recoveries at spike levels of 100 and 150% of the declared amount were 99.0% with a relative standard deviation (RSD) of 2.1%, and 101% with an RSD of 2.3%, respectively. The test results between laboratories on each commercial product were reproducible with RSD values of no more than 4.0%, and the results were repeatable in the same laboratory with an average RSD of 0.7%. HorRat values ranged from 0.5 to 1.7 on both tests of spike recovery and reproducibility between laboratories on commercial products. The average determination coefficient of the calibration curves from the laboratories was 0.9995 with an RSD of 0.03%. All of the 12 collaborating laboratories succeeded in the study and none of their reported test results were outliers, partly indicating the robustness of the method. It is recommended that the method be accepted by AOAC INTERNATIONAL as Official First Action.

Opinion of the safety of glucosamine hydrochloride from Aspergillus niger as food ingredient

“…The Cargill laboratory was one of 12 laboratories that participated in the Association of Official Agricultural Chemists (AOAC) ring study that was conducted on the AOAC glucosamine assay method (AOAC Official Method 2005.01). All 12 of the laboratories succeeded in the study and none of the reported test results were outliers (Zhou et al, 2005). Arsenic, heavy metals, residual solvents and microbiological testing are conducted by the National Food Laboratory, Inc.…”

Optimization and validation of spectrophotometric determination of glucosamine in dosage Form with sodium 1,2-naphthoquinone-4-sulphonate

“…Several published methods described the determination of Glucosamine (GL) in dosage forms. These methods include spectrophotometry (Wu et al 2005;Yamaguchi et al 2004;Burtseva et al 1986) , high -performance liquid chromatography (HPLC) (Hadad et al 2012;Zang et al 2006;Niu et al 2006;Tekko et al 2006;Eberendu et al 2005;Zhou et al 2005;Shen et al 2005;Ji et al 2005), TLC-densitometry (Esters et al 2006;Sullivan et al 2005), and capillary electrophoresis (Qi et al 2006;Garcia and Henry. 2005).…”

“…The developed method is direct, sensitive, accurate and highly cost-effective for routine studies when compared to HPLC (Hadad et al 2012;Zang et al 2006;Niu et al 2006;Tekko et al 2006;Eberendu et al 2005;Zhou et al 2005;Shen et al 2005;Ji et al 2005) and other techniques such as capillary electrophoresis (Qi et al 2006;Garcia and Henry. 2005).…”

Comparison of Active Ingredient Consistency of Some Brand and Generically Available Glucosamine Products in Iranian Pharmacies

“…Glucosamine products in Iran pharmacies are presented in various prices. Different content ranges which were revealed in previous studies determined these products in Iran and other countries [10][11][12][13][14]. Even in a study by Adebowal et al in university of Maryland percent of label claim less than 10% for chondroitin and less than 40% for Glucosamine were reported [15].…”

“…According to final FDA rules, GMP for dietary supplement were published that ensures production quality, contamination and labels accuracy [10,24]. But deviation from label value had been demonstrated different ranges among several studies that determined Glucosamine products even as sulphate form [11][12][13][14]. In addition Glucosamine and chondroitin content of commercial products, as products evaluated in this study wasn't relevant to their prices [14,25,26].…”