Main Article Content
Abstract
Method verification is one of the steps required to ensure that all methods used meet the standards required for data reliability and accuracy in a laboratory that implements Good Laboratory Practices (GLP). In accordance with ISO 16140-3:2021, the method verification for microbiology testing implemented by calculating the Intralaboratory Reproducibility Standard Deviation (SIR) for implementation verification and eBias value for food item verification. Method verification for enumeration of Enterobacteriaceae in food products using ISO 16140-3 has never been carried out at the Indonesian Food and Drug Authority (FDA) laboratories. Therefore, verification of this method needs to be performed. This study aimed to verify the ISO 21528-2:2017 as reference method for enumeration of Enterobacteriaceae in food products by colony count technique. The selected food item for implementation verification was pasteurized milk while for food item verification, the selected food items were yogurt, traditional preserved egg (telur pindang), sweet and hard candy, seasoning dry powder, worcester sauce and cassava chips. All of selected foods were artificially contaminated with Escherichia coli WDCM 00012. The SIR value obtained was 0.12 ≤ 2× 0,18 (lowest mean value of SR from ISO 21528-2:2017), indicating that the acceptability limit for the implementation verification was met. While the eBias value for all selected food item were less than 0,5 log10, thus the verification study in the National Quality Contol Laboratory of Drug and Food (NQCLDF), Indonesian FDA, meets the acceptance criteria defined in the standard ISO 16140-3:2021.
Keywords
Article Details
References
- Belouafa, S., Habti, F., Benhar, S., Belafkih, B., Tayane, S., Hamdouch, S., Bennamara, A., & Abourriche, A. (2017). Statistical tools and approaches to validate analytical methods: methodology and practical examples. International Journal of Metrology and Quality Engineering, 8, 9. https://doi.org/10.1051/ijmqe/2016030.
- Baylis C., Han Joosten, M.U., & Davie, A. 2011. Enterobacteriaceae and their significance to the food industry. ILSI Europe Report Series. http://www.innocua.net/web/download-1053/ep-enterobacteriaceae.pdf.
- Ellison, S.L.R, Key, P & Wood, R (2012). The Interlaboratory Performance of Microbiological Methods for Food Analysis. Journal of AOAC International, 95(5), 1433-1439. DOI: 10.5740/jaoacint.11-452.
- Faridah, D. N., Erawan, D., Sutriah, K., Hadi A., & Budiantari, F. (2018). Implementasi SNI ISO/IEC 17025:2017 Persyaratan Umum Kompetensi Laboratorium Pengujian dan Laboratorium Kalibrasi. Badan Standardisasi Nasional, Jakarta.
- Feinberg, M., D. Sohier., and Jean-Francois David. (2009). Validation of an Alternative Method for Counting Enterobacteriaceae in Foods Based on Accuracy Profile. Journal of AOAC International Vol. 92, No.2, 527-537.
- Halkman, H. B. D., & Halkman, A. K. (2014). Indicator Organisms. In Encyclopedia of Food Microbiology (pp. 358–363). Elsevier. https://doi.org/10.1016/B978-0-12-384730-0.00396-7
- Hoorfar, J. (2011). Rapid detection, characterization, and enumeration of foodborne pathogens. APMIS, 119(s133), 1–24. https://doi.org/10.1111/j.1600-0463.2011.02767.x
- Indonesian FDA. (2019). Regulation No.13. 2019: Maximum Limit of Microbial Contaminants in Processed Food (pp. 1–48).
- International Organization for Standardization (ISO). (2017a). ISO 21528: 2017. Microbiology of the food chain — Horizontal method for the detection and enumeration of Enterobacteriaceae — Part 2: Colony-count technique.
- International Organization for Standardization (ISO). (2017b). ISO/IEC 17025: 2017. General requirements for the competence of testing and calibration laboratories. .
- International Organization for Standardization (ISO). (2019). ISO 19036: 2019. Microbiology of the food chain - Estimation of measurement uncertainty for quantitative determinations. .
- International Organization for Standardization (ISO). (2021). ISO 16140-3:2021. Microbiology of the food chain - Method validation - Part 3: Protocol for the validation of alternative (proprietary) methods against a reference method. International Organization for Standardization, Geneva.
- Khezri, M., Khanzadi, S., & Hashemi, M. (2022). Determination of Performance Characteristics (eLOD50) for Verification of Qualitative Food Microbiological Measurement Methods Based on EN ISO 16140-3:2021. Research Square, 1–11.
- Leclercq, A. (2002). Flexibilization of the scope of accreditation: an important asset for food and water microbiology laboratories. Accreditation and Quality Assurance, 7(7), 299–304. https://doi.org/10.1007/s00769-002-0494-7
- Lombard B. (2010). ISO Standardization and Validation of Reference Testing Methods Validation of Alternative Methods in Food Microbiology. Jpn. J. Food Microbiol, 27(1), 8–20.
- Lombard, B., & Leclercq A. (2010). The role of standardization bodies in the harmonization of analytical methods in Food Microbiology. In Global Issues in Food Science and Technology (pp. 177–197).
- Lombard, B., & Leclercq, A. (2011). Validation of Innovative Food Microbiological Methods According to the EN ISO 16140 Standard. Food Analytical Methods, 4(2), 163–172. https://doi.org/10.1007/s12161-010-9154-4.
- Paulsen, P., C. Borgetti, E. Schopf, and J.M. Smulders. (2008). Enumeration of Enterobacteriaceae in Various Foods with a New Automated Most-Probable-Number Method Compared with Petrifilm and International Organization for Standardization Procedures. Journal of Food Protection, Vol. 71, No. 2, 376–379.
- Sandle, T. (2015). Approaching Microbiological Method Validation. IVT, 1–19.
- Silbernagel, K. M., and K. G. Lindberg. (2002). Evaluation of the 3M Petrifilm Enterobacteriaceae count plate method for the enumeration of Enterobacteriaceae in foods. J. Food Prot. 65:1452–1456
References
Belouafa, S., Habti, F., Benhar, S., Belafkih, B., Tayane, S., Hamdouch, S., Bennamara, A., & Abourriche, A. (2017). Statistical tools and approaches to validate analytical methods: methodology and practical examples. International Journal of Metrology and Quality Engineering, 8, 9. https://doi.org/10.1051/ijmqe/2016030.
Baylis C., Han Joosten, M.U., & Davie, A. 2011. Enterobacteriaceae and their significance to the food industry. ILSI Europe Report Series. http://www.innocua.net/web/download-1053/ep-enterobacteriaceae.pdf.
Ellison, S.L.R, Key, P & Wood, R (2012). The Interlaboratory Performance of Microbiological Methods for Food Analysis. Journal of AOAC International, 95(5), 1433-1439. DOI: 10.5740/jaoacint.11-452.
Faridah, D. N., Erawan, D., Sutriah, K., Hadi A., & Budiantari, F. (2018). Implementasi SNI ISO/IEC 17025:2017 Persyaratan Umum Kompetensi Laboratorium Pengujian dan Laboratorium Kalibrasi. Badan Standardisasi Nasional, Jakarta.
Feinberg, M., D. Sohier., and Jean-Francois David. (2009). Validation of an Alternative Method for Counting Enterobacteriaceae in Foods Based on Accuracy Profile. Journal of AOAC International Vol. 92, No.2, 527-537.
Halkman, H. B. D., & Halkman, A. K. (2014). Indicator Organisms. In Encyclopedia of Food Microbiology (pp. 358–363). Elsevier. https://doi.org/10.1016/B978-0-12-384730-0.00396-7
Hoorfar, J. (2011). Rapid detection, characterization, and enumeration of foodborne pathogens. APMIS, 119(s133), 1–24. https://doi.org/10.1111/j.1600-0463.2011.02767.x
Indonesian FDA. (2019). Regulation No.13. 2019: Maximum Limit of Microbial Contaminants in Processed Food (pp. 1–48).
International Organization for Standardization (ISO). (2017a). ISO 21528: 2017. Microbiology of the food chain — Horizontal method for the detection and enumeration of Enterobacteriaceae — Part 2: Colony-count technique.
International Organization for Standardization (ISO). (2017b). ISO/IEC 17025: 2017. General requirements for the competence of testing and calibration laboratories. .
International Organization for Standardization (ISO). (2019). ISO 19036: 2019. Microbiology of the food chain - Estimation of measurement uncertainty for quantitative determinations. .
International Organization for Standardization (ISO). (2021). ISO 16140-3:2021. Microbiology of the food chain - Method validation - Part 3: Protocol for the validation of alternative (proprietary) methods against a reference method. International Organization for Standardization, Geneva.
Khezri, M., Khanzadi, S., & Hashemi, M. (2022). Determination of Performance Characteristics (eLOD50) for Verification of Qualitative Food Microbiological Measurement Methods Based on EN ISO 16140-3:2021. Research Square, 1–11.
Leclercq, A. (2002). Flexibilization of the scope of accreditation: an important asset for food and water microbiology laboratories. Accreditation and Quality Assurance, 7(7), 299–304. https://doi.org/10.1007/s00769-002-0494-7
Lombard B. (2010). ISO Standardization and Validation of Reference Testing Methods Validation of Alternative Methods in Food Microbiology. Jpn. J. Food Microbiol, 27(1), 8–20.
Lombard, B., & Leclercq A. (2010). The role of standardization bodies in the harmonization of analytical methods in Food Microbiology. In Global Issues in Food Science and Technology (pp. 177–197).
Lombard, B., & Leclercq, A. (2011). Validation of Innovative Food Microbiological Methods According to the EN ISO 16140 Standard. Food Analytical Methods, 4(2), 163–172. https://doi.org/10.1007/s12161-010-9154-4.
Paulsen, P., C. Borgetti, E. Schopf, and J.M. Smulders. (2008). Enumeration of Enterobacteriaceae in Various Foods with a New Automated Most-Probable-Number Method Compared with Petrifilm and International Organization for Standardization Procedures. Journal of Food Protection, Vol. 71, No. 2, 376–379.
Sandle, T. (2015). Approaching Microbiological Method Validation. IVT, 1–19.
Silbernagel, K. M., and K. G. Lindberg. (2002). Evaluation of the 3M Petrifilm Enterobacteriaceae count plate method for the enumeration of Enterobacteriaceae in foods. J. Food Prot. 65:1452–1456