Determination of 26 anti-diabetic compounds in dietary supplements using a validated UPLC method

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Mar;35(3):387-394. doi: 10.1080/19440049.2017.1332429. Epub 2017 Dec 28.

Abstract

The purpose of this study was to validate a rapid, simple and accurate method using ultra-performance liquid chromatography (UPLC) for the simultaneous determination of 26 anti-diabetic compounds in illegally adulterated dietary supplements. The method was validated for specificity, linearity, limit of detection, limit of quantitation, precision, accuracy, recovery and stability. All compounds were separated with a resolution of over 1.5. The limits of detection and quantitation were 0.10-1.70 and 0.30-5.10 µg g-1 in a solid sample, respectively; the corresponding values were 0.10-1.25 and 0.30-3.75 µg ml-1 in a liquid sample. The correlation coefficient was > 0.99, precisions were 0.11-3.30% (intra-day) and 0.05-6.15% (inter-day), and accuracies were 83-108% (intra-day) and 85-109% (inter-day). The recoveries were measured with six dosage forms, and the results were acceptable as 87-117% with relative standard deviations ≤ 6.44%. The relative standard deviations of stability were ≤ 3.40% and the standard solution was stable for 48 h. Ninety-six samples were obtained from on/off-line markets and were analysed using the developed method. Among these samples, pioglitazone and glibenclamide were found in seven samples and the concentrations of each compound were 0.15% and 0.26-0.51%, respectively. With the increasing adulteration of dietary supplements with anti-diabetic drugs, this method may be helpful to protect public health and safety.

Keywords: Determination; anti-diabetes; dietary supplements; monitoring; simultaneous analysis; ultra-performance liquid chromatography; validation.

MeSH terms

  • Chromatography, High Pressure Liquid
  • Dietary Supplements / analysis*
  • Drug Contamination
  • Hypoglycemic Agents / analysis*
  • Reproducibility of Results

Substances

  • Hypoglycemic Agents