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Clearwater, FL, United States

Zhang W.,Synutra Research Laboratory | Giancaspro G.,United States Pharmacopeial Convention | Adams K.M.,United States Pharmacopeial Convention | Neal-Kababick J.,Flora Research Laboratories | And 4 more authors.
Journal of AOAC International | Year: 2014

The most commonly used chondroitin sulfate (CS) assay method is cetylpyridinium chloride (CPC) titration. Cellulose acetate membrane electrophoresis (CAME) is the technique used for detection of impurities in the U.S. Pharmacopeia's CS monograph. Because CPC titration is a relatively nonspecific quantitative technique, the apparent amount of CS as determined by CPC titration alone may not reflect the true amount of CS due to possible interference with the CPC assay by impurities that contain CPC titratable functional groups. When CAME is used in conjunction with CPC titration, certain non-CS and adulterants can be visualized and estimated, and a true value for CS can be assigned once the presence of these non-CS impurities has been ruled out. This study examines conjunct application of CPC and CAME in ascertaining CS assay and purity in the presence of certain adulterants. These include propylene glycol alginate sulfate sodium, known in commerce as alginic sodium diester (ASD), and Zero One (Z1), a water-soluble agent newly reported in the CS marketplace and subsequently identified as sodium hexametaphosphate. ASD, Z1, and CS are similar in physical appearance and solubility in water and ethanol. They are also titratable anions and form ionic pairs with CPC, therefore interfering with the CPC titration assay for CS. CAME separates these adulterants from each other and from CS by differences in their electrophoretic mobility. CAME is able to detect these impurities in CS at levels as low as 0.66% by weight. Although it is recommended that a method for detecting impurities (e.g., CAME) be used in combination with relatively nonspecific assay methods such as CPC titration, this is seldom done in practice. Assay results for CS derived from CPC titration may, therefore, be misleading, leaving the CS supply chain vulnerable to adulteration. In this study, the authors investigated ASD and Z1 adulteration of CS and developed an electrophoretic separation of these adulterants in CS and procedures to isolate ASD from CS matrixes containing these adulterants. The authors describe in this paper utilization of an orthogonal approach to establish the identity of Z1 as sodium hexametaphosphate and to confirm the identity of ASD, including ethanol fractionation, FTIR spectroscopy, differential scanning calorimetry, and NMR spectroscopy. The authors suggest that CAME is a cost-effective and easy to use method for detecting certain impurities in CS raw ingredients and recommend that CPC and CAME be used in combination by QC laboratories as a means of effectively deterring the practice of adulterating CS raw materials with the known adulterants ASD and Z1 and/or other non-chondroitin substances that can be separated from CS by CAME and that exhibit CPC titration behavior similar to CS. Source

Kupina S.,Constellation Research | Roman M.,Tampa Bay Analytical Research
Journal of AOAC International | Year: 2014

An international collaborative study was conducted of an HPLC-refractive index (RI) detector method for the determination of the combined amounts of sugars, glycerol, organic acids, and phenolic compounds in wines and wine-like beverages. Nine collaborating laboratories representing major winery, contract laboratories, and government laboratories tested eight different materials as blind duplicates using the proposed method. Sample materials included red and white wines, port, wine cooler, and nonalcoholic wine. One material was a negative control, and one material was a reference material. Samples were either treated with an ion-exchange resin to remove interfering organic acids prior to analysis or left untreated to include organic acids and phenolics. Red wine samples were treated with polyvinylpolypyrrolidone to remove potential interferences from phenolics prior to analysis. The HPLC analyses were performed on a Bio-Rad Fast Acid Analysis Column using RI detection. Reproducibility (RSDR) for untreated samples (sugars + phenolics + organic acids) ranged from 6.6% for Titrivin AA4 reference material to 11.0% for dry red wine. RSDR for treated samples (sugars only) ranged from 6.8% for white zinfandel to 18.9% for dry white wine. RSDR for treated samples (sugars only) + glycerol ranged from 6.4% for white zinfandel to 19.8% for dry red wine. Based on these results, the method was adopted as Official First Action status for determination of total carbohydrates in wine and wine-like beverages. © 2014 Publishing Technology. Source

Roman M.C.,Tampa Bay Analytical Research | Hildreth J.,Blaze Science Industries | Bannister S.,Hightower Pharmaceutical Services Corporation
Journal of AOAC International | Year: 2013

A rapid method has been developed to quantify seven catechins and caffeine in green tea (Camillia sinensis) raw material and powdered extract, and dietary supplements containing green tea extract. The method utilizes RP HPLC with a phenyl-based stationary phase and gradient elution. Detection is by UV absorbance. The total run time, including column re-equilibration, is 13 min. Single-laboratory validation (SLV) has been performed on the method to determine the repeatability, accuracy, selectivity, LOD, LOQ, ruggedness, and linearity for (+)-catechin, (-)-epicatechin, (-)-epicatechin gallate, (-)- epigallocatechin, (-)-gallocatechin gallate, (-)-epigallocatechin gallate, and (+)-gallocatechin, as well as caffeine. Repeatability precision and recovery results met AOAC guidelines for SLV studies for all catechins and caffeine down to a level of approximately 20 mg/g. Finished products containing high concentrations of minerals require the use of EDTA to prevent decomposition of the catechins. © 2014 Publishing Technology. Source

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