Accreditation and Quality Assurance

, Volume 24, Issue 1, pp 79–84 | Cite as

Provision of proficiency testing for histamine mass fraction in canned tuna to improve the capability of chemical laboratories in the Philippines

  • Benilda S. EbarviaEmail author
  • Aaron Dacuya
  • Sharlene R. Cabanilla
  • Natividad R. Mamplata
Practitioner's Report


In this work, two reference materials (RMs) for mass fraction of histamine in canned tuna were developed to address the need of local testing laboratories for matrix RMs and a PT scheme for histamine. A validated method using HPLC with fluorescence detector (340 nm for excitation and 445 nm for emission) was applied with post-column derivatization for the RM’s homogeneity and stability studies. Acceptable results were obtained after statistical evaluation of homogeneity and stability according to IUPAC Harmonized Protocol and ISO Guide 35, respectively. Two PT exercises for histamine determination based on ISO/IEC 17043 were organized in 2014 and 2015 with the assigned values of 148 and 65 mg/kg, respectively. These reference values were obtained using exact matching liquid chromatography–isotope dilution mass spectrometry (LC–IDMS) with gravimetric sample preparation. The corresponding uncertainty of the reference value was obtained by ISO GUM approach where the characterization of the sample gave the highest contribution (41 %). The satisfactory z-score performance evaluated from the 12 laboratories was 50 % and 58.3 % in the first and second PT round, respectively. Most of the laboratories used AOAC Official Method 977.13 but not all conducted method validation. The 50 % decrease in unsatisfactory results in the second PT round is a significant improvement in the local laboratory performance for histamine analysis. However, the provision of more PT schemes and the increased use of CRMs in the future are still needed by these laboratories for external quality assurance and method validation to enhance the present capability.


Proficiency testing Histamine Reference material Reference value Exact matching LC–IDMS 



The funding support from the Department of Science and Technology (DOST) and the Philippine Council for Industry, Energy and Emerging Technology Research and Development (PCIEERD) is greatly acknowledged.


  1. 1.
    Onal A (2007) A review: current analytical methods for the determination of biogenic amines in foods. Food Chem 103:1475–1486CrossRefGoogle Scholar
  2. 2.
    RASFF – Food and Feed Safety Alerts (2014) European commission. Accessed 8 Nov 2014
  3. 3.
    PNS ISO Guide 34 (2010) General requirements for the competence of reference material producers. Bureau of Product Standards, PhilippinesGoogle Scholar
  4. 4.
    ISO/IEC 17043 (2010) Conformity assessment: general requirements for proficiency testing. International Organization for Standardization (ISO), GenevaGoogle Scholar
  5. 5.
    Official Methods of Analysis of AOAC International (2005) Official Method 977.13, 18th edn. AOAC International, Gaithersburg, MD, USAGoogle Scholar
  6. 6.
    Custodio FB, Tavares E, Gloria MBA (2007) Extraction of bioactive amines from grated Parmesan cheese using acid, alkaline and organic solvents. J Food Compos Anal 20:280–288CrossRefGoogle Scholar
  7. 7.
    Byrd N (2013) Quick, easy and reliable detection of histamine in food using the agilent 6490 triple quadrupole LC/MS with jet stream technology. Accessed 24 Nov 2014
  8. 8.
    Official Methods of Analysis of AOAC International (2005) Appendix F: guidelines on method performance requirements, 18th edn. AOAC International, Gaithersburg, MD, USAGoogle Scholar
  9. 9.
    Thompson M, Ellison SLR, Wood R (2006) The international harmonized protocol for the proficiency testing of analytical chemistry laboratories (IUPAC technical report). Pure Appl Chem 78:145–196CrossRefGoogle Scholar
  10. 10.
    PNS ISO Guide 35 (2010) Reference materials: general and statistical principles for certification. Bureau of Product Standards, PhilippinesGoogle Scholar
  11. 11.
    Lee I, Ahn S, Kim B, Hwang E, Kim YS (2008) Analysis of benzoic acid in quasi-drug drink using isotope dilution liquid chromatoraphy mass spectrometry. Bull Korean Chem Soc 29:2125–2128CrossRefGoogle Scholar
  12. 12.
    Shin H, Kim B, Lee J, Hwang E (2010) Development of an isotope-dilution liquid chromatography/mass spectrometric method for the accurate determination of acetaminophen in tablets. Bull Korean Chem Soc 31:3663–3667CrossRefGoogle Scholar
  13. 13.
    Vogl J, Fritzkow W (2010) Isotope dilution mass spectrometry: a primary method of measurement and its role for RM certification. MAPAN J Metrol Soc India 25:135–164Google Scholar
  14. 14.
    Joint Committee Guides in Metrology (2008) JCGM 100:2008 Evaluation of measurement data - Guide to the expression of uncertainty in measurement (GUM 1995 with minor corrections). 1st Ed., SèvresGoogle Scholar
  15. 15.
    ISO 13258 (2005) Statistical methods for use in proficiency testing by interlaboratory comparisons. International Organization for Standardization (ISO), GenevaGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Benilda S. Ebarvia
    • 1
    Email author
  • Aaron Dacuya
    • 1
  • Sharlene R. Cabanilla
    • 1
  • Natividad R. Mamplata
    • 1
  1. 1.Department of Science and Technology-Industrial Technology Development Institute (DOST-ITDI)Taguig CityPhilippines

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