Quantitative Analysis of Aloins and Aloin-Emodin in Aloe Vera Raw Materials and Finished Products Using High-Performance Liquid Chromatography: Single-Laboratory Validation, First Action 2016.09

Abstract Single laboratory validation of a method for determination of glucosamine in raw materials and dietary supplements containing glucosamine sulfate and/or glucosamine hydrochloride by with high-performance liquid chromatography FMOC-Su derivatization. Tests with 2 blank matrixes containing SAMe, vitamin C, citric acid, chondroitin sulfates, methylsulfonylmethane, lemon juice concentrate, and other potential interferents showed the method to be selective and specific. Eight calibration curves prepared over 7 working days indicated excellent reproducibility with the linear range at least over 2.0–150 μg/mL, and determination coefficients >0.9999. Average spike recovery from the blank matrix (n = 8 over 2 days) was 93.5, 99.4, and 100.4% at respective spike levels of 15, 100, and 150%, and from the sample matrix containing glucosamine (n = 3) was 99.9 and 102.8% at respective levels of 10 and 40%, with relative standard deviations <0.9%. The method was also applied to 12 various glucosamine finished products and raw materials. The stability tests confirmed that glucosamine–FMOC-Su derivative once formed is stable at room temperature for at least 5 days. Limit of quantitation was 1 μg/mL and limit of detection was 0.3 μg/mL. The method is ready to proceed for the collaborative study.

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Determination of Major Phenolic Compounds in Echinacea spp. Raw Materials and Finished Products by High-Performance Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation Matrix Extension

Journal of AOAC International ◽

10.5740/jaoacint.11-142 ◽

2011 ◽

Vol 94 (5) ◽

pp. 1400-1410 ◽

Cited By ~ 26

Author(s):

Paula N. Brown ◽

Michael Chan ◽

Lori Paley ◽

Joseph M. Betz

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Phenolic Compounds ◽

High Performance ◽

Raw Materials ◽

Ultraviolet Detection ◽

Matrix Extension ◽

Single Laboratory

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Determination of Ubidecarenone (Coenzyme Q10, Ubiquinol-10) in Raw Materials and Dietary Supplements by High-Performance Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation

Journal of AOAC International ◽

10.1093/jaoac/90.5.1227 ◽

2007 ◽

Vol 90 (5) ◽

pp. 1227-1236 ◽

Cited By ~ 8

Author(s):

Debra Orozco ◽

Jules Skamarack ◽

Kelly Reins ◽

Barry Titlow ◽

Steve Lunetta ◽

...

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Dietary Supplements ◽

Coenzyme Q10 ◽

High Performance ◽

Raw Materials ◽

Biologically Active ◽

Ultraviolet Detection ◽

Relative Standard ◽

Single Laboratory

Abstract A method based on high-performance liquid chromatography with ultraviolet detection has been developed to quantify ubidecarenone [coenzyme Q10 (CoQ10)] in raw materials and dietary supplements. Single-laboratory validation has been performed on the method to determine repeatability, accuracy, selectivity, limits of detection and quantification (LOQ), ruggedness, and linearity for CoQ10. As CoQ10 can exist as the biologically active reduced form, the application of an oxidizing agent, ferric chloride, drives the equilibrium mechanics to the fully oxidized state and allows for exact quantification of total CoQ10 in the sample. This method was found to be fit and linear for the testing of materials containing CoQ10 in the range of 501000 mg/g. Repeatability precision for CoQ10 was between 2.15 and 5.00 relative standard deviation. Observed recovery of CoQ10 was found to be between 93.8 and 100.9. LOQ was found to be 9 g/mL. Further, limited studies showed that some adulterants and degraded material could be satisfactorily separated from CoQ10 and identified.

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