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

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    Detection of phenobarbital adulteration in dietary supplements: simultaneous analysis of 16 sedative-hypnotics and sleep-inducers by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS)

    Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
    2019, v.32 no.1, pp.24-34
    https://doi.org/10.5806/AST.2019.32.1.24
    Ji Hyun Lee (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Ji Yeon Choi (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Hanna Park (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Ah Young Min (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Nam Sook Kim (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Seong Soo Park (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Sung-Kwan Park (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
    Ho-il Kang (Division of Advanced Analysis, National Institute of Food and Drug Safety Evaluation, Ministry of Food &)
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    Abstract

    The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of 16 sedative-hypnotics and sleep inducers in dietary supplements was determined by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS). The UPLC method was validated, providing a linearity (R2) of more than 0.999, and LODs and LOQs that ranged from 0.2 to 0.5 and 0.6 to 1.5 μg mL−1, respectively. The repeatabilities were 0.2-8.4 % (intra-day) and 0.3-4.5 % (inter-day), and the accuracies were 89.0-117.0 % (intra-day) and 87.8-111.9 % (inter-day). The mean recoveries of the spiked samples ranged from 98.7 to 107.3 %. The relative standard deviation (%RSD) of the stability was less than 2.4 %. Using the developed method, one sedative-hypnotic compound, phenobarbital, was detected in one of the nineteen samples tested. In addition, the major characteristic fragment ions of each target compound were confirmed using Q-Orbitrap-MS for higher accuracy. Monitoring the presence of these 16 sedative-hypnotics and sleep inducers in dietary supplements should be pursued in the interest of human health, and the results of this study confirmed that the developed method has value for this application.

    keywords
    Sedative-Hypnotics, Adulterants, UPLC-UV, Q-Orbitrap-MS, Method Validation


    Reference

    1

    1. Q. Gao, B. Che, Z. Zhang, H. Dai, and H. Guo, J. Chin. Pharm. Univ., 39, 142-146 (2008).

    2

    2. B. Zhu, Z. Zhao, Z. Wang, Q. Xue, and L. Zhao, Chin. J. Pharm. Anal., 30, 745-751 (2010).

    3

    3. J. Liu, L. Xiao, X. Guan, Y. Xiong, T. Wang, and J. Li, Chin. J. Pharm. Anal., 31, 376-379 (2011).

    4

    4. P. Jin, Z. Wang, W. Wang, D. Zou, J. Ma, and X. Hu, Chin Pharm. J., 47, 462-466 (2012).

    5

    5. L. J. Greenfield, S. H. Zaman, M. L. Sutherland, S. C. Lummis, M. I. Niemeyer, E. A. Barnard, and R. L. Macdonald, Neuropharmacology, 42, 502-521 (2002).

    6

    6. C. Gottesmann, Neuroscience, 111, 231-239 (2002).

    7

    7. J. Wang, B. Chen, and S. Yao, Food addit. Contam., 25, 822-830 (2008).

    8

    8. Z. Wang, J. Zhang, and Y. Zhang, J. Chin. Mass Spec. Soc., 30, 282-286 (2009).

    9

    9. A. Yan, X. Li, C. Xi, L. Zhang, S. Xia, G. Wang, B. Tang, and Z. Mu, Chinese J. Anal. Chem., 41, 509-516(2013).

    10

    10. E. Deconinck, P. Y. Sacré, P. Courselle, and J. O. De Beer, J. Chromatogr. Sci., 51, 791-806 (2013).

    11

    11. AOAC Official Methods of Analysis. Internationalconference on harmonization of harmonized tripartiteguideline, validation of analytical procedures: text andmethodology.

    12

    12. AOAC International, Rockville, MD (2005).

    13

    13. ICH International conference on Harmonization. Harmonized tripartite guideline, validation of analyticalprocedures:text and methodology Q2

    14

    14. (R1). European Medicines Agency (EUMA), London, UK .

    15

    15. A, El-Gindy, Il Farmaco, 60, 745 (2005).

    16

    16. R. A. Menck, D. S. De Lima, S. C. Seulin, V. Leyton, C. A. Pasqualucci, D. R. Munoz, M. D. Osseltore, M. Yonamine, J. Sep. Sci., 35, 3361-3368 (2012).

    17

    17. X. Zhang, Z. Lin, J. Li, Z. Huang, Y. Rao, H. Liang, J. Yan, and F. Zheng. Drug Testing and Analysis, 9, 588-595 (2017).

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