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Monitoring of purity and stability of CRMs of multiclass pesticides during prolonged storage before and after expiration

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Abstract

Certified reference materials (CRMs) are the backbone for qualitative and quantitative determination of pesticides in technical materials, formulations, and food matrices. However, their stringent expiry date, limited shelf life, and diminishing purity with time, limits their use beyond expiry. Stability study of 89 CRMs of multiclass pesticides, stored at − 25 °C, has been conducted to assess the purity of CRMs beyond their expiry date. It was evident that > 96 % of the CRMs remained optimally stable with respect to their observed purity even after their expiry date as per certificate of analysis. Percentage deviations in purity of expired and valid CRMs posited well below 7 % and are within ± 10 % acceptable range as recommended by the SANTE. During 2013–2017, performance of the valid and expired CRMs was evaluated through 44 z-scores obtained in 14 international and national proficiency testing programmes. All the z-scores received for 15 expired and 29 valid CRMs were found satisfactory. Inter-laboratory comparison of 6 randomly selected expired and valid CRMs was tested at three different ISO/IEC 17025 accredited laboratories and their % difference between purities ranged from − 2.35 % to + 0.95 %. It was inferred that by maintaining proper storage conditions and continuous monitoring of purity, the expired CRMs can give comparable results as valid CRMs.

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References

  1. Armishaw P (2016) Certified reference materials—a path to traceable chemical measurements. Department of Industry, Innovation and Science, National Measurement Institute, 5 May 2016, 1–26. https://www.easurement.gov.au. Accessed 24 Oct 2018

  2. BIPM, IEC, IFCC, ILAC, ISO, IUPAC, IUPAP and OIML (2012) International vocabulary of metrology—Basic and general concepts and associated terms (VIM), 3rd edn. JCGM 200:2012. BIPM. https://www.bipm.org/utils/common/documents/jcgm/JCGM_200_2012.pdf. Accessed 25 Sept 2019

  3. ISO/IEC 17025 (2005) General requirements for the competence of calibration and testing laboratories, 2nd edn. International Organization for Standardization (ISO), Geneva, Switzerland

    Google Scholar 

  4. Reenie M (2015) Parris. Panel 11: reference materials and proficiency tests. Certified reference materials and proficiency tests: Provision, production, and value assignment. National Institute of Standards and Technology (NIST), USA. 11 Dec 2015, pp 1–76 http://www.resag.org.br/congressoresag2015/anais/img/pdfs/20160301092315.pdf. Accessed 24 Oct 2018

  5. ISO 17034 (2016) General requirements for the competence of reference material producers. International Organization for Standardization (ISO), Geneva, Switzerland

    Google Scholar 

  6. ISO Guide 30 (2015) Reference materials-selected terms and definitions. International Organization for Standardization (ISO), Geneva, Switzerland

    Google Scholar 

  7. ISO Guide 31 (2015) Reference materials-contents of certificates, labels and accompanying documentation. International Organization for Standardization (ISO), Geneva, Switzerland

    Google Scholar 

  8. ISO Guide 35 (2017) Reference materials-guidance for characterization and assessment of homogeneity and stability. International Organization for Standardization (ISO), Geneva, Switzerland

    Google Scholar 

  9. De Biévre P, Dybkaer R, Fajgelj A, Hibbert DB (2011) Metrological traceability of measurement results in chemistry: concepts and implementation (IUPAC Technical Report). Pure Appl Chem 83(10):1873–1935

    Article  Google Scholar 

  10. Guimarães EF, do Rego ECP, Cunha HCM, Rodrigues JM, Figueroa-Villar JD (2014) Certified reference material for traceability in environmental analysis: pAHs in toluene. J Braz Chem Soc 25(2):351–360

    Google Scholar 

  11. Rettinger M, Sreenivasan U, Dilek I, Pogue S (2010) What makes a good reference standard? Cerilliant analytical reference standard. Cerilliant Corporation, Round Rock, pp 1–32

    Google Scholar 

  12. Pauwels J, Lamberty A, Schimmel H (1998) Quantification of the expected shelf-life of certified reference materials. Fresenius’ J Anal Chem 361(5):395–399

    Article  CAS  Google Scholar 

  13. Lamberty A, Schimmel H, Pauwels J (1998) The study of the stability of reference materials by isochronous measurements. Fresenius’ J Anal Chem 360:359–361

    Article  CAS  Google Scholar 

  14. SANTE (2017) Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed. SANTE/11813/2017, 21–22 November 2017 rev.0, European Commission Directorate General for Health and Food Safety, Bruxelles/Brussel, Belgium, pp 1–46

  15. WHO (2006a) WHO standardization. Recommendations for the preparation, characterization and establishment of international and other biological reference standards (revised 2004). WHO technical report series 2006, no. 932

  16. WHO (2006b) WHO working group on stability of reference materials for biological medicines and in vitro diagnostics. Geneva, Switzerland, 27–28 November 2006, pp 1–15

  17. Tahlan A, Barrowcliffe T, Das RG, Shin J, Wood D (2005) WHO technical workshop on stability of reference materials for biological medicines and in vitro diagnostics, Geneva, Switzerland, 28–29 November 2005. Biologicals 2007

  18. Thompson M (2016) Analytical methods committee, AMCTB no. 74: z-scores and other scores in chemical proficiency testing-their meanings, and some common misconceptions. Anal Methods 8:5553–5555

    Article  Google Scholar 

  19. ISO 13528 (2015) Statistical methods for use in proficiency testing by inter-laboratory comparison. International Organization for Standardization (ISO), Geneva

  20. Cunningham WC, Capar SG (2014) Elemental analysis manual for food and related products. Elemental analysis manual (Section 3.5 reference materials). FDA, US Food and Drug Administration, US Department of Health and Human Services, USA. 1–9 http://www.fda.gov/Food/FoodScienceResearch/LaboratoryMethods/ucm2006954.html. Accessed 24 Oct 2018

  21. Roelandts I, Gladney ES (1998) Consensus values for NIST biological and environmental standard reference materials. Fresenius’ J Anal Chem 360:327–338

    Article  CAS  Google Scholar 

  22. ISO Guide 34 (2009) General requirements for the competence of reference material producers. International Organization for Standardization (ISO), Geneva

  23. ISO/IEC 17043 (2010) Conformity assessment—general requirements for proficiency testing. International Organization for Standardization (ISO), Geneva

  24. Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multi-residue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. J AOAC Int 86:412–431

    Article  CAS  Google Scholar 

  25. Wu J, Lu J, Wilson C, Lin Y, Lu H (2010) Effective liquid-liquid extraction method for analysis of pyrethroid and phenylpyrazole pesticides in emulsion-prone surface water samples. J Chromatogr A 1217(41):6327–6333

    Article  CAS  Google Scholar 

  26. National Measurement Institute (NMI) (2016) Proficiency test report AQA 15–16 Cocaine. January 2016. National Measurement Institute, Department of Industry, Innovation and Science, Australian Government, pp 1–30

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Acknowledgements

This work was supported by ICAR—Indian Council of Agricultural Research and Department of Agriculture, Cooperation and Farmers Welfare, Ministry of Agriculture, Government of India, New Delhi, India.

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Authors and Affiliations

  1. Project Coordinating Cell, Pesticide Residue Laboratory, All India Network Project on Pesticide Residues, ICAR—Indian Agricultural Research Institute, New Delhi, 110 012, India

    Krishan Kumar Sharma, Vandana Tripathy, Rahul Gautam, Ruchi Gupta, Amol Tayade, Khushbu Sharma, Rajbir Yadav, Poonam Shukla, Suneeta Devi, Priya Pandey, Gitansh Singh, Shobhita Kalra & Suresh Walia

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  1. Krishan Kumar Sharma
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Correspondence to Krishan Kumar Sharma.

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Sharma, K.K., Tripathy, V., Gautam, R. et al. Monitoring of purity and stability of CRMs of multiclass pesticides during prolonged storage before and after expiration. Accred Qual Assur 25, 89–97 (2020). https://doi.org/10.1007/s00769-019-01411-w

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  • DOI: https://doi.org/10.1007/s00769-019-01411-w

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