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  • P-ISSN 1225-0163
  • E-ISSN 2288-8985

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    Vol.32, No.2
    PubReader Citation Share

    Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample

    Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
    2019, v.32 no.2, pp.35-47
    https://doi.org/10.5806/AST.2019.32.2.35
    Nam Sook Kim (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Geum Joo Yoo (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Kyu Yeon Kim (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Ji Hyun Lee (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Sung-Kwan Park (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Sun Young Baek (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Hoil Kang (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food and)
    Nam, S. K. , Geum, J. Y. , Kyu, Y. K. , Ji, H. L. , Sung-Kwan, P. , Sun, Y. B. , & Hoil, K. (2019). Development and validation of an LC-MS/MS method for the simultaneous analysis of 26 anti-diabetic drugs in adulterated dietary supplements and its application to a forensic sample. Analytical Science and Technology, 32(2), 35-47, https://doi.org/10.5806/AST.2019.32.2.35
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    Abstract

    In this study, high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS/ MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak® C18 MGII (2.0 mm × 100 mm, 3 μm), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with R2 > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively

    keywords
    adulteration, antidiabetes drugs, dietary supplement, LC-MS/MS, validation, monitoring


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