Efficient production of reference materials of hazardous organics using smart calibration by nuclear magnetic resonance

  • Takeshi SaitoEmail author
  • Toshihide Ihara
  • Tooru Miura
  • Yuuko Yamada
  • Koichi Chiba
General Paper


The accurate quantification of pesticide residues in food is an important factor in assuring the quality of life of our citizens. In general, chromatographic methods are used, which require certified reference materials (CRMs) for each analyte of interest for accurate quantitative analysis. Recently, regulation of pesticides in food, limiting the positive maximum residue (positive list system) has been brought into effect in Japan. Furthermore, ISO/IEC 17025 requires calibration and testing laboratories to program calibrations and measurements traceable to the International System of Units (SI). Accordingly, these laboratories need a suite of CRMs that are traceable to the SI. In order to address these requirements for every analyte of interest in an efficient manner, a new approach to producing SI traceable CRMs is required. Nuclear magnetic resonance (NMR) has been used widely in chemical analysis. One of the well known characteristics of NMR is the proportional relationship between peak area and the number of nuclei contributing to the peak. If accurate relative intensities of peak areas are obtained, this provides an attractive quantitative tool for organic compounds. The area of a signal from an analyte can be measured with respect to another signal originating from a comparator that has been added to the sample solution. The chosen comparator should not react with the analyte or resonate at any chemical shift similar to that of the analyte. This enables us to produce SI traceable CRMs more effectively. In this paper, we demonstrate a new approach for producing CRMs for pesticides using quantitative NMR—an SI traceable quantitative technique.


Nuclear magnetic resonance Quantification Purity Calibration Traceability Pesticide Reference material 


  1. 1.
    Introduction of the Positive List Systems for Agricultural Chemical Residues in Food (2006) Department of food safety, ministry of health, labor and welfare, Tokyo, Japan. Accessed 1 April 2011
  2. 2.
    ISO Guide 30: 1992/Amendment 1: 2008 (2008) Terms and definitions used in connection with reference materials/Amendment 1. Revision of definitions for reference material and certified reference material. ISO, Geneva, SwitzerlandGoogle Scholar
  3. 3.
    Saito T, Ihara T, Koike M, Kinugasa S, Fujimine Y, Nose K, Hirai T (2009) Accred Qual Assur 14:79–86CrossRefGoogle Scholar
  4. 4.
    Pauli GF, Jaki BU, Lankin DC (2007) J Nat Prod 70:589–595CrossRefGoogle Scholar
  5. 5.
    Kontogianni VG, Exarchou V, Troganis A, Gerothanassis I (2009) Anal Chim Acta 635:188–195CrossRefGoogle Scholar
  6. 6.
    Diehl BWK, Malz F, Hlozgrabe U (2007) Spectroscopy Eur 19:15–19Google Scholar
  7. 7.
    Wells RJ, Cheung J, Hook JM (2004) Accred Qual Assur 9:450–456CrossRefGoogle Scholar
  8. 8.
    Malz F, Jancke H (2006) Anal Bioanal Chem 385:760–765CrossRefGoogle Scholar
  9. 9.
    Malz F, Jancke H (2005) J Pharm Biomed Anal 38:813–823CrossRefGoogle Scholar
  10. 10.
    Griffiths L, Irving AM (1998) Analyst 123:1061–1068CrossRefGoogle Scholar
  11. 11.
    Saito T, Nakaie S, Kinoshita M, Ihara T, Kinugasa S, Nomura A, Maeda T (2004) Metrologia 41:213–218CrossRefGoogle Scholar
  12. 12.
    Al-Deen TS, Hibbert DB, Hook JM, Wells RJ (2004) Accred Qual Assur 9:55–63CrossRefGoogle Scholar
  13. 13.
    Jancke H, Malz F, Haesselbarth W (2005) Accred Qual Assur 10:421–429CrossRefGoogle Scholar
  14. 14.
    Ihara T, Saito T, Sugimoto N (2009) Synthesiology 2:13–24CrossRefGoogle Scholar
  15. 15.
    Shaka AJ, Barker PB, Freeman R (1985) J Magn Reson 64:547–552Google Scholar
  16. 16.
    Fujiwara T, Anai T, Nagayama K (1993) J Magn Reson A 104:103–105CrossRefGoogle Scholar
  17. 17.
    Coplen TB, Böhlke JK, De Bièvre P, Ding T, Holden NE, Hopple JA, Krouse HR, Lamberty A, Peiser HS K, Révész K, Rieder SE, Rosman KJR, Roth E, Taylor PDP, Vocker RD Jr, Xiao YK (2002) Pure Appl Chem 74:1987–2017CrossRefGoogle Scholar
  18. 18.
    ISO/IEC Guide 98-3: 2008 (2008) Uncertainty of measurement—Part 3: Guide to the expression of uncertainty in measurement (GUM: 1995), ISO/IEC, SwitzerlandGoogle Scholar
  19. 19.
    ISO/IEC Guide 99:2007 (2007) International vocabulary of meteorology—basic and general concepts and associated terms (VIM)—3rd ed, ISO/IEC, SwitzerlandGoogle Scholar
  20. 20.
    Palermo EF, Chiu J (1976) Thermochim Acta 14:1–12CrossRefGoogle Scholar
  21. 21.
    Milton MJT, Quinn TJ (2001) Metrologia 38:289–296CrossRefGoogle Scholar

Copyright information

© Springer-Verlag 2011

Authors and Affiliations

  • Takeshi Saito
    • 1
    Email author
  • Toshihide Ihara
    • 1
  • Tooru Miura
    • 1
  • Yuuko Yamada
    • 2
  • Koichi Chiba
    • 1
  1. 1.National Metrology Institute of JapanAISTTsukubaJapan
  2. 2.Wako Pure Chemical IndustriesKawagoeJapan

Personalised recommendations