ANALYTICAL VALIDATION OF CLOPIDOGREL IN HUMAN PLASMA THROUGH ULTRAHIGHPERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

Authors

  • Yahdiana Harahap Department of Pharmacy, Faculty of Pharmacy, Universitas Indonesia, Depok, Indonesia.
  • Innet Maysyarah Department of Pharmacy, Faculty of Pharmacy, Universitas Indonesia, Depok, Indonesia.

DOI:

https://doi.org/10.22159/ijap.2017.v9s1.79_86

Keywords:

Clopidogrel, Irbesartan, Optimization, Liquid chromatography-tandem mass spectrometry, Validation

Abstract

Objective: This study developed a sensitive, selective, and valid method for analyzing clopidogrel in human plasma using liquid chromatographytandem
mass spectrometry (LC-MS/MS).
Methods: The chromatography separation was performed on the waters ACQUITY UPLC Class BEH C18 1.7 μm (2.1 × 100 mm) column, consisting of
0.1% formic acid in water and 0.1% formic acid in acetonitrile (30-70) as the mobile phase, and an isocratic elution with a flow rate of 0.2 mL/minutes.
The mass detection was performed using a Waters Xevo TQD equipped with positive electrospray ionization in the multiple reaction monitoring
modes. The clopidogrel was detected at m/z 322.086>212.097 and irbesartan as an internal standard at m/z 429.233>207.131. The sample was
prepared with protein precipitation method using acetonitrile, vortex mixed for 10 minutes, and centrifuged at 13,000 rpm for 20 minutes.
Results: This method showed a linear result at the concentration range of 0.2-10 ng/ml with r≥0.9997.
Conclusions: The developed method provides sensitivity, linearity, precision, and accuracy and is suitable for analysis of clopidogrel in human plasma
using LC-MS/MS.

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References

Dipiro JT, Talbert RL, Yee GC, Matzke GR, Wells BG, Posey LM.

Pharmacotherapy A Pathophysiologic Approach. 3rd ed. New York: The

McGraw-Hill Companies. Inc.; 2008.

Brunton LL, Chabner B, Knollmann BC, editors. Goodman & Gilman’s

the Pharmacological Basis of Therapeutics. New York: McGraw-Hill

Medical; 2011.

Robinson A, Hillis J, Neal C, Leary AC. The validation of a bio

analytical method for the determination of clopidogrel in human plasma.

J Chromatogr B Analyt Technol Biomed Life Sci 2007;848(2):344-54.

Nirogi RV, Kandikere VN, Shukla M, Mudigonda K, Maurya S,

Boosi R. Quantification of clopidogrel in human plasma by sensitive

liquid chromatography/tandem mass spectrometry. Rapid Commun

Mass Spectrom 2006;20(11):1695-700.

Shin BS, Yoo SD. Determination of clopidogrel in human plasma by

liquid chromatography/tandem mass spectrometry: Application to a

clinical pharmacokinetic study. Biomed Chromatogr 2007;21(9):883-9.

European Medicines Agency. CHMP efficacy working party

therapeutic subgroup on pharmacokinetics (EWP-PK). Guideline on

the Investigation of Bioequivalence (Draft). London: An Agency of the

European Union; 2008.

European Medicines Agency. CHMP efficacy working party

therapeutic subgroup on pharmacokinetics (EWP-PK). Guideline on the

Investigation of Bioequivalence. London: An Agency of the European

Union; 2010.

Food and Drug Administration. Guidance for Industry: Bioanalytical

Method Validation. United States of America: Department of Health

and Human Services; 2013.

Karazniewicz-Lada M, Danielak D, Tezyk A, Zaba C, Tuffal G,

Glówka F. HPLC-MS/MS method for the simultaneous determination

of clopidogrel, its carboxylic acid metabolite and derivatized isomers

of thiol metabolite in clinical samples. J Chromatogr B Analyt Technol

Biomed Life Sci 2012;911:105-2.

Kruve A, Leito I. Comparison of different methods aiming to account

for/overcome matrix effects in LC/ESI/MS on the example of pesticide

analyses. Anal Methods 2013;5:3035-44.

Henriques ST, Castanho MA. Environmental factors that enhance the

action of the cell penetrating peptide pep-1 a spectroscopic study using

lipidic vesicles. Biochim Biophys Acta 2005;1669(2):75-86.

Marangon E, Posocco B, Mazzega E, Toffoli G. Development and

validation of a high-performance liquid chromatography-tandem mass

spectrometry method for the simultaneous determination of irinotecan

and its main metabolites in human plasma and its application in a

clinical pharmacokinetic study. PLoS One 2015;10(2):e0118194.

Fig. 4: Representative multiple reaction monitoring chromatograms of the plasma blank

Int J App Pharm, Special Issue (October) Harahap et al.

Ciaffoni L, Hancock G, Harrison JJ, van Helden JP, Langley CE,

Peverall R, et al. Demonstration of a mid-infrared cavity enhanced

absorption spectrometer for breath acetone detection. Anal Chem

;85(2):846-50.

Chico J, Holthoon F, Zuidema T. Ion suppression study for tetracyclines in feed. Chromatogr Res Int 2012;2012:135854.

Panuwet P, Hunter RE Jr, D’Souza PE, Chen X, Radford SA,

Cohen JR, et al. Biological matrix effects in quantitative tandem mass

spectrometry-based analytical methods: Advancing biomonitoring. Crit Rev Anal Chem 2016;46(2):93-105.

Published

30-10-2017

How to Cite

Harahap, Y., & Maysyarah, I. (2017). ANALYTICAL VALIDATION OF CLOPIDOGREL IN HUMAN PLASMA THROUGH ULTRAHIGHPERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY. International Journal of Applied Pharmaceutics, 9, 163–167. https://doi.org/10.22159/ijap.2017.v9s1.79_86

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