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International Guidelines for Bioanalytical Method Validation: A Comparison and Discussion on Current Scenario

Abstract

US FDA released guidelines for bioanalytical method validation in 2001 and it became the basis for guidelines such as ANVISA and EMA. Even though there is a general agreement between these guidelines in terms of evaluation of validation parameters, significant diversity exists with respect to methodology employed. Present review compares and summarizes the regulatory guidelines issued by US FDA, ANVISA and EMA for bioanalytical method validation. This review also discusses evaluation of certain validation parameters such as matrix effect, incurred sample reanalysis, various stability aspects, effect of anticoagulant counter ions, specificity in the presence of concomitant medications, and identification of pharmacokinetic repeats wherein specific guidance and general consensus amongst scientific community does not exist.

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Abbreviations

AAPS:

American Association of Pharmaceutical Scientists

ANVISA:

The National Health Surveillance Agency

CC:

Calibration curve

CV:

Coefficient of variation

CVG:

Calibration and validation group

DL:

Detection limit

DoE:

Design of experimentation

EDTA:

Ethylenediaminetetraacetic acid

EMA:

European Medicines Agency

GLP:

Good Laboratory Practices

HQC:

Higher quality control sample

IS:

Internal Standard

ISR:

Incurred Sample Reanalysis

LOD:

Limit of detection

LOQ:

Limit of quantification

LLOQ:

Lower limit of quantification

LLOQQC:

Quality control sample at lower limit of quantification

MF:

Matrix factor

MQC:

Middle quality control sample

QC:

Quality control sample

RSD:

Residual standard deviation

ULOQ:

Upper limit of quantification

US FDA:

United States Food and Drug Administration

References

  1. Shah VP, Midha KK, Dighe S, McGilveray IJ, Skelly JP, Yacobi A, Layloff T, Viswanathan CT, Cook CE, McDowall RD, Pittman KA, Spector S (1992) Pharm Res 9(4):588–592

    Article  Google Scholar 

  2. Food and Drug Administration (1999) Draft Guidance for Industry: Bioanalytical Method Validation. Rockville, MD, US Food and Drug Administration, Center for Drug Evaluation and Research

  3. Shah VP, Midha KK, Findlay JW, Hill HM, Hulse JD, McGilveray IJ, McKay G, Miller KJ, Patnaik RN, Powell ML, Tonelli A, Viswanathan CT, Yacobi A (2000) Pharm Res 17(12):1551–1557

    CAS  Article  Google Scholar 

  4. Food and Drug Administration (2001) Guidance for Industry: Bioanalytical method validation. US Food and Drug Administration, Center for Drug Evaluation and Research, Rockville

  5. Viswanathan CT, Bansal S, Booth B, DeStefano AJ, Rose MJ, Sailstad J, Shah VP, Skelly JP, Swann PG, Weiner R (2007) AAPS J 9(1):E30–E42

    Article  Google Scholar 

  6. Agência Nacional de Vigilância Sanitária (2003) Guide for validation of analytical and bioanalytical methods. Resolution - RE n. 899

  7. European Medicines Agency (2009) Guideline on Validation of Bioanalytical Methods. Committee for Medicinal Products for Human Use, London

  8. Garofolo F (2001) The 1st Canadian Workshop on the Crystal City AAPS/FDA White Paper. Workshop Report. http://www.canadianlcmsgroup.com/docs/B-2007WorkshopWhitePaper.pdf. Accessed on 29 July 2010

  9. Savoie N, Booth BP, Bradley T, Garofolo F, Hughes NC, Hussain S, King SP, Lindsay M, Lowes S, Ormsby E, Phull R, Rocci ML, Vallano PT, Viau A, Zhu Z (2009) Bioanalysis 1(1):19–30

    CAS  Article  Google Scholar 

  10. Savoie N, Garofolo F, van Amsterdam P, Booth BP, Fast DM, Lindsay M, Lowes S, Masse R, Mawer L, Ormsby E, Phull R, Rocci ML, Vallano PT, Yin X (2010) Bioanalysis 2(1):53–68

    CAS  Article  Google Scholar 

  11. Aboul-Enein HY (2000) Accredit Qual Assur 5(5):180–181

    CAS  Article  Google Scholar 

  12. Bolton S (1997) Pharmaceutical statistics: practical and clinical application. Marcel Dekker, New York

  13. Almeida AM, Castel-Branco MM, Falcao AC (2002) J Chromatogr B 774(2):215–222

    CAS  Article  Google Scholar 

  14. Hartmann C, Smeyers-Verbeke J, Massart DL, McDowall RD (1998) J Pharm Biomed Anal 17:193–218

    CAS  Article  Google Scholar 

  15. Wieling J, Hendriks G, Tamming WJ, Hempenius J, Mensink CK, Oosterhuis B, Jonkman JH (1996) J Chromatogr A 730(1–2):381–394

    CAS  Article  Google Scholar 

  16. Heyden YV, Nijhuis A, Smeyers-Verbeke J, Vandeginste BGM, Massart DL (2001) J Pharm Biomed Anal 24(5–6):723–753

    Article  Google Scholar 

  17. Bende G, Kollipara S, Kolachina V, Saha R (2007) Chromatographia 66(11–12):859–866

    CAS  Article  Google Scholar 

  18. International Conference on Harmonization (1996) Note for guidance on validation of analytical procedures: methodology, the tripartite harmonised ICH guideline, Topic Q2B

  19. Karnes HT, Shiu G, Shah VP (1991) Pharm Res 8(4):421–426

    CAS  Article  Google Scholar 

  20. Hoffman D, Kringle R, Singer J, McDougall S (2009) J Chromatogr B 877:2262–2269

    CAS  Article  Google Scholar 

  21. Hughes NC, Wong EYK, Fan J, Bajaj N (2007) AAPS J 9(3):E353–E360

    CAS  Article  Google Scholar 

  22. King R, Bonfiglio R, Fernandez-Metzler C, Miller-Stein C, Olah T (2000) J Am Soc Mass Spectrom 11(11):942–950

    CAS  Article  Google Scholar 

  23. Chambers E, Wagrowski-Diehl DM, Lu Z, Mazzeo JR (2007) J Chromatogr B 852:22–34

    CAS  Article  Google Scholar 

  24. Matuszewski BK (2006) J Chromatogr B 830(2):293–300

    CAS  Article  Google Scholar 

  25. Matuszewski BK, Constanzer ML, Chavez-Eng CM (2003) Anal Chem 75(13):3019–3030

    CAS  Article  Google Scholar 

  26. Wang S, Cyronak M, Yang E (2007) J Pharm Biomed Anal 43(2):701–707

    CAS  Article  Google Scholar 

  27. Fast DM, Kelley M, Viswanathan CT, O’Shaughnessy J, King SP, Chaudhary A, Weiner R, DeStefano AJ, Tang D (2009) AAPS J 11(2):238–241

    Article  Google Scholar 

  28. Bergeron M, Bergeron A, Furtado M, Garofolo F (2009) Bioanalysis 1(3):537–548

    CAS  Article  Google Scholar 

  29. Pharm PK Discussion—Different bioanalytical methods for Fasting and Fed study. http://www.boomer.org/pkin/PK09/PK2009119.html. Accessed on 30 July 2010

  30. King SP, Aungst BJ, Shen HSL (2009) Bioanalysis 1(8):1415–1418

    CAS  Article  Google Scholar 

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Correspondence to Jyoti Paliwal.

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Kollipara, S., Bende, G., Agarwal, N. et al. International Guidelines for Bioanalytical Method Validation: A Comparison and Discussion on Current Scenario. Chromatographia 73, 201–217 (2011). https://doi.org/10.1007/s10337-010-1869-2

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  • DOI: https://doi.org/10.1007/s10337-010-1869-2

Keywords

  • Bioanalysis
  • Validation
  • US FDA
  • ANVISA
  • EMA
  • Regulatory guidance