Open Access
CC BY-NC-ND 4.0 · Ibnosina Journal of Medicine and Biomedical Sciences 2012; 04(02): 44-52
DOI: 10.4103/1947-489X.210755
Article

Identification of prednisolone, methylprednisolone and their metabolites in human urine using HPLC (+) ESI-MS/MS and detection of possible adulteration in Indian herbal drug preparations

Authors

  • Ahi Shobha

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003
  • Dubey Sachin

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003
  • Upadhyay Awanish

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003
  • S Yadav

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003
  • Rakesh Rakesh

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003
  • Priyadarshi Rahul

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003
  • Beotra Alka

    National Dope Testing Laboratory (NDTL) JN Stadium Complex, East Gate, CGO, Lodhi Road, New Delhi, India 110003

Objective: To explore the possibility of identifying the maximum number of metabolites of prednisolone and methylprednisolone by LC-MS/MS and to further test the application of this developed method on six Indian herbal drug preparations. Method and Materials: The sample extraction procedure involves enzymatic hydrolysis and liquid-liquid extraction and further analysis using LC-MS/ MS. The excretion profile was performed with four healthy male volunteers after administration of 40 mg and 8 mg of prednisolone and methylprednisolone, respectively. Six herbal drug preparations obtained from All India Institute of Medical Sciences, India were tested to detect the possible adulteration with prednisolone or methylprednisolone. Results: The Analytical method was validated as per the requirement of WADA International Standard of Laboratories (version 6.0). The parent compound and ten urinary metabolites of prednisolone could be identified. The parent, M-1, M-2 and M-3 could be detected up to 72 hours while rest of the metabolites were detectable up to 24 hours. In the case of methylprednisolone, the parent compound and six urinary metabolites were identified. M-1 and M-2 of methylprednisolone were detectable up to 48 hours while the parent drug methylprednisolone and other metabolites were detectable up to 24 hours. Out of the six herbal drugs tested, one showed the presence of prednisolone. Conclusion: The improved detection method developed for the identification and detection of prednisolone and methylprednisolone metabolites would prove highly beneficial in extending the time of detection of drug abuse in athletes and also detecting spiked ayurvedic, homeopathic and unani preparations.



Publication History

Received: 15 October 2011

Accepted: 26 December 2011

Article published online:
23 May 2022

© 2012. The Author(s). This is an open access article published by Thieme under the terms of the Creative Commons Attribution-NonDerivative-NonCommercial License, permitting copying and reproduction so long as the original work is given appropriate credit. Contents may not be used for commercial purposes, or adapted, remixed, transformed or built upon. (https://creativecommons.org/licenses/by-nc-nd/4.0/)

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