jrnls.org logo
Submit

BROWSE ALL JOURNALS

SEE ALL 19 JOURNALS
Indian Journal of Pharmaceutical Education and ResearchNOW IN
Article

Method Development and Validation for Detection of Procaterol in Human Urine using Gas Chromatography-Tandem Mass Spectrometry

Shila Jain1, Puran Lal Sahu1, Srashti Raj2, Abhinav Shrivastava1, Ashok Kumar Maurya1, Rajiv Kumar Tonk2, Kapendra Sahu1★★ Corresponding author

  1. 1National Dope Testing Laboratory, Ministry of Youth Affairs and Sports (MYAS), Government of India, New Delhi, INDIA.
  2. 2Delhi Pharmaceutical Sciences and Research University, M.B. Road, New Delhi, INDIA.

CORRESPONDENCE

Kapendra Sahu

National Dope Testing Laboratory, Ministry of Youth Affairs and Sports (MYAS), Government of India, New Delhi, INDIA.

kapendra_sahu@yahoo.com

Received: 21-04-2019; Revised: 04-09-2019; Accepted: 06-11-2019.

Volume 54, Issue 1 · pp. 150–154 · PUBLISHED 2020 · DOI: 10.5530/ijper.54.1.18

View on IJPER original site ↗

ABSTRACT

Background: A simple, sensitive and accurate method for the determination of procaterol in human urine was developed and validated using Gas Chromatography coupled to tandem mass spectrometry (GC-MS/MS) as per the requirements of World Anti-Doping Agency (WADA) and ICH guidelines. Methodology: The sample processing includes deconjugation with enzymatic hydrolysis, Solid Phase Extraction (SPE) procedure using XAD2 column and Liquid-liquid Extraction (LLE) followed by the derivatisation using N-methyl trimethylsilysl trifluoroacetamide (MSTFA). Results: The method included a chromatographic run of 17 min and the calibration curve was linear over the concentration range of 5-40 ng/mL with a correlation coefficient (r) of 0.98. The intra- and inter-day assay precision ranged from 0.75 to 0.94% and 1.2 to 1.70%, respectively. The absolute recovery percentage for procaterol was found to be 83%. The recovery was sufficient to reliable identify the procaterol at or below the level prescribed by WADA ie MRPL 20ng/ ml. The LOQ and LOD was found to be 5 and 3 ng/ml respectively. Conclusion: A simple and sensitive GC-MS/MS method for quantitative estimation of Procaterol was developed and validated as per the WADA ISL and ICH guidelines. This developed method could be also used for therapeutic drug monitoring purposes.

KEYWORDS

Open in new tab

REFERENCES

As published

Showing references and in-text citations exactly as published.

    Cite this article

    SELECT FORMAT

    Jain, S., Sahu, P. L., Raj, S., Shrivastava, A., Maurya, A. K., Tonk, R. K., & Sahu, K. (2020). Method Development and Validation for Detection of Procaterol in Human Urine using Gas Chromatography-Tandem Mass Spectrometry. Indian Journal of Pharmaceutical Education and Research, 54(1), 150–154. https://doi.org/10.5530/ijper.54.1.18