Acta Univ. Agric. Silvic. Mendelianae Brun. 2013, 61(6), 1669-1679 | DOI: 10.11118/actaun201361061669

Evaluation of development in indirect determination of milk fat free fatty acids in Czech Republic

Oto Hanuš1, Eva Samková2, Jan Říha1, Marcela Vyletělová Klimešová1, Petr Roubal1
1 Dairy Research Institute, Ltd., Prague, Ke Dvoru 12a, 160 00 Praha 6 - Vokovice, Czech Republic
2 University of South Bohemia České Budějovice, Branišovská 1, 370 05 České Budějovice, Czech Republic

Free fatty acids (FFAs) in fat are important indicator of raw milk quality. Result reliability of FFAs is important. Aim was to verify MIR-FT (mid infrared spectroscopy with Fourier's transformations) method for its calibration to determine FFAs, time stability of MIR-FT FFA calibration and calibration levelling in laboratory networks. Reference (RE) milk samples (1 set = 8) were prepared according to CSN 57 0533 (FFAs in mmol.100g-1 of fat). MIR-FT instruments were: 1 LactoScope FTIR (DE); 2 Bentley FTS (BE); 2 MilkoScan FT 6000 (FO). 3 calibrations of MIR-FT (5) in 3 laboratories were performed. Bulk milk samples came from 4 herds and 2 breeds. These 4 samples were used for calibration in native and modified form. Modification increased FFAs by cca 100%. Calibration set had 8 samples. 1 between calibration interval was checked monthly by proficiency testing (PT). PT set had 10 samples. 5 samples were with native milk and 5 had modified fat content, lower and higher. Maximal value of difference variability for calibration quality validation is x (sd of difference MIR-FT and RE) plus 1.64 multiple of sd (on 95% level), 1.0613 mmol.100g-1. Mean validation correlation coefficient (r) between MIR-FT and RE results was 0.802 ± 0.082 (P < 0.001), from 0.666 to 0.945. Minimal value at calibration is x minus 1.64 multiple of sd (0.668). Correlations between MIR-FT results were higher by 8.4% (0.869 (P < 0.001) > 0.802). Example PT with 10 and 5 milk samples had similar results of r 0.887 and 0.953 (P < 0.001 and P < 0.05). There is possibility to construct a levelling programme for calibrated instruments. Some equation between PT reference and instrumental values could correct MIR-FT results for their better comparability.

Keywords: raw cow milk quality, fat, reference, titration, infrared spectroscopy, stability of calibration, result reliability, proficiency testing, result levelling
Grants and funding:

This paper was supported by projects Ministry of Agriculture No NAZV KUS QJ1210301, RO0513 from February 2013 and NAZV QH81105 and Ministry of Education, Youth and Sports No MSM 6007665806.

Received: May 11, 2021; Published: November 24, 2013  Show citation

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Hanuš, O., Samková, E., Říha, J., Vyletělová Klimešová, M., & Roubal, P. (2013). Evaluation of development in indirect determination of milk fat free fatty acids in Czech Republic. Acta Universitatis Agriculturae et Silviculturae Mendelianae Brunensis, 61(6), 1669-1679. doi: 10.11118/actaun201361061669
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    References

    1. ANTONELLI, M. L., CURINI, R., SCRICCIOLO, D., VINCI, G., 2002: Determination of free fatty acids and lipase activity in milk: quality and storage markers. Talanta, 58: 561-568. ISSN 0039-9140. DOI: 10.1016/S0039-9140(02)00324-7 Go to original source...
    2. BIJGAART VAN DEN, H., 2006: New applications of mid-infra-red spectrometry for the analysis of milk and milk products. 2 Free fatty acids. IDF Bulletin, 406: 22-28. ISSN 0250-5118.
    3. CEMPÍRKOVÁ, R., 2007: Contamination of cow's raw milk by psychrotrophic and mesophilic microflora in relation to selected factor. Czech J. Anim. Sci., 52, 11: 387-393. ISSN 1212-1819. DOI: 10.17221/2325-CJAS Go to original source...
    4. CEMPÍRKOVÁ, R., 2002: Psychrotrophic vs. total bacterial counts in bulk milk samples. Vet. Med.-Czech, 47, 8: 227-233. ISSN 0375-8427. DOI: 10.17221/5829-VETMED Go to original source...
    5. CEMPÍRKOVÁ, R., 2001: The technology of dairy cows breeding in relation to the hygienic quality of milk. (In Czech) Coll. Sci. Pap. Fac. Agric. in České Budějovice, Ser. Anim. Sci., 18, 1: 33-46. ISSN 1212-558X.
    6. CEMPÍRKOVÁ, R., MIKULOVÁ, M., 2009: Incidence of psychrotrophic lipolytic bacteria in cow's raw milk. Czech J. Anim. Sci., 54, 2: 65-73. ISSN 1212-1819. DOI: 10.17221/1667-CJAS Go to original source...
    7. CEMPÍRKOVÁ, R., MIKULOVÁ, M., TRÁVNÍČEK, J., 2009: Counts of psychrotrophic lipolytic bacteria in cow's raw milk samples from the aspect of technological quality. J. Agrobiol., 26, 2: 113-121. ISSN 1803-4403.
    8. CEMPÍRKOVÁ, R., THÉR, R., 2000: The effect of living conditions on selected indexes of raw cow's milk. (In Czech) Coll. Sci. Pap. Fac. Agric. in České Budějovice, Ser. Anim. Sci., 17, 1: 55-71. ISSN 1212-558X.
    9. CVAK, Z., PETERKOVÁ, L., ČERNÁ, E., 1992: Chemical and physic-chemical methods in milk and dairy product quality control. (In Czech). Praha: VÚP, Milcom servis a.s. Praha, (118) 222. ISBN 80-85120-36-4.
    10. CSN 57 0529, 1993: Raw cow milk for dairy factory treatment and processing. Praha, ČNI.
    11. CSN 57 0533, 1997: Milk - determination of matter content of free fatty acids. ČNI Prague.
    12. DANKOW, R., WOJTOWSKI, J., FAHR, R. D., 2004: Hygienic quality of raw milk in relation to methods of production and storage. Med. Wet., 60: 46-49. ISSN 0025-8628.
    13. DEETH, H. C., 2006: Lipoprotein lipase and lipolysis in milk. Inter. Dairy J., 16: 555-562. ISSN 0958-6946. DOI: 10.1016/j.idairyj.2005.08.011 Go to original source...
    14. FERLAY, A., MARTIN, B., PRADEL, P., COULON, J. B., CHILLIARD, Y., 2006: Influence of grass-based diets on milk fatty acid composition and milk lipolytic system in Tarentaise and Montbeliarde cow breeds. J. Dairy Sci., 89: 4026-4041. ISSN 0022-0302. DOI: 10.3168/jds.S0022-0302(06)72446-8 Go to original source...
    15. FOLTYS, V., KIRCHNEROVÁ, K., 2006: Mesophilic and psychrotrophic aerobe sporulating microorganisms in raw cow's milk. Centr. Eur. J. Biol., 1: 545-560. ISSN 1895-104X. DOI: 10.2478/s11535-006-0037-z Go to original source...
    16. FOLTYS, V., KIRCHNEROVÁ, K., 2010: Occurence and detection of aerobic sporulating microorganisms in raw cow's milk. Slovak J. Anim. Sci., 43, 2: 83-87. ISSN 1337-9984.
    17. FOSS, 2001: MilkoScan FT 6000; Free fatty acids measurement (FFA). Spectrum Calibration.
    18. FOSS, 2004: MilkoScan FT 120; Improved milk calibration. Analytical Application Note No. 128e.
    19. GENČUROVÁ, V., HANUŠ, O., JEDELSKÁ, R., KOPECKÝ, J., 2011: Creation and development of the calibration model for the indirect determination of milk fat free fatty acids and the method of a reference sample preparation. (In Czech) Výzkum v chovu skotu / Cattle Research, LIII, 193, 1: 10-20. ISSN 0139-7265.
    20. GENČUROVÁ, V., HANUŠ, O., KUČERA, J., SOJKOVÁ, K., KOPECKÝ, J., JEDELSKÁ, R., 2009: Free fatty acids as possible indicator for milk quality improvement. Acta fytotech. zootech., 12: 25-28. ISSN 1335-258X.
    21. GRAPPIN, R., 1987: Definition and evaluation of the overall accuracy of indirect methods of milk analysis - aplication to calibration procedure and quality control in dairy laboratory. Bulletin of the International Dairy Federation, Doc. 208, IDF Provisional Standard 128: 3-12. ISSN 0250-5118.
    22. GRAPPIN, R., 1993: European network of dairy laboratories. In: Proceedings of an International Analytical Quality Assurance and Good Laboratory Practice in Dairy Laboratories. Sonthofen / Germany: 205-211, 1992-05-18/20, Brussels.
    23. HANTIS-ZACHAROV, E., HALPERN, M., 2007: Culturable psychrotrophic bacteria communities in raw milk and their proteolytic and lipolytic traits. Appl. Environ. Microbiol., 73: 7162-7168. ISSN 0099-2240. DOI: 10.1128/AEM.00866-07 Go to original source...
    24. HANUŠ, O., FRELICH, J., VYLETĚLOVÁ, M., ROUBAL, P., VORLÍČEK, Z., JEDELSKÁ, R., 2004: Technologically difficult, pathogenic and food risky bacterial contamination of raw milk and other materials from dairy cow herds. Czech J. Anim. Sci., 49, 11: 489-499. ISSN 1212-1819. DOI: 10.17221/4336-CJAS Go to original source...
    25. HANUŠ, O., GENČUROVÁ, V., KOPECKÝ, J., JEDELSKÁ, R., MOTYČKA, Z., ČERNOCKÝ, M., 2008 a: The interpretation of experimental calibration results of routine IR instruments for determination of free fatty acid contents of milk fat. (In Czech) Výzkum v chovu skotu / Cattle Research, L, 182, 2: 55-62. ISSN 0139-7265.
    26. HANUŠ, O., KUČERA, J., GENČUROVÁ, V., KOPECKÝ, J., JEDELSKÁ, R., 2009: Selected parameters of MIR-FT method validation to measurement of free fatty acids in milk fat for milk quality laboratories. (In Czech) Výzkum v chovu skotu / Cattle Research, LI, 187, 3: 27-34. ISSN 0139-7265.
    27. HANUŠ, O., VEGRICHT, J., FRELICH, J., MACEK, A., BJELKA, M., LOUDA, F., JANŮ, L., 2008 b: Analyse of raw cow milk quality according to free fatty acids contents in the Czech Republic. Czech J. Anim. Sci., 53, 1: 17-30. ISSN 1212-1819. DOI: 10.17221/2717-CJAS Go to original source...
    28. IDF, 1991: Determination of free fatty acids in milk and milk products. IDF Bulletin No. 256, Brussels, International Dairy Federation.
    29. KERKHOF MOGOT, M. F., KOOPS, J., NEETER, R., SLANGEN, K. J., HEMERT VAN, H., KOOYMAN, O., WOOLDRIK, H., 1982: Routine testing of farm tank milk with the Milko-Scan 203. 1. Calibration procedure and small-scale experiments. Neth. Milk Dairy J., 36: 115-133. ISSN 0958-6946.
    30. KOOPS, J., KLOMP, H., HEMERT VAN, H., 1990: Rapid enzymatic assay of free fatty acids (lipolysis) in farm tank milk by a segmented continuous-flow method. Comparison of the results with those obtained by the BDI procedure. Neth. Milk Dairy J., 44: 3-19. ISSN 0958-6946.
    31. LERAY, O., 1993: CECALAIT: an organization to support analytical quality assurance in dairy laboratories. Proceedings of an International Analytical Quality Assurance and Good Laboratory Practice in Dairy Laboratories. Sonthofen / Germany: 349-360, 1992-05-18/20, Brussels.
    32. LERAY, O., 2006: Reference and calibration system for routine milk testing - advantages / disadvantages, choice criteria. 3rd ICAR reference laboratory network meeting - Kuopio, Finland - 6th June, 49-65. Breeding, production recording, health and the evaluation of farm animals. EAAP publication No. 121, 2007, Proceedings of the 35th biennial session of ICAR: 311-317. ISBN 978-90-8686-030-2.
    33. MA, Y., RYAN, C., BARBANO, D. M., GALTON, D. M., RUDAN, M. A., BOOR, K. J., 2000: Effects of somatic cell count on quality and shelf-life of pasteurized fluid milk. J. Dairy Sci., 83: 264-274. ISSN 0022-0302. DOI: 10.3168/jds.S0022-0302(00)74873-9 Go to original source...
    34. MIKULOVÁ, M., 2011: Content of free fatty acids lipolytic bacteria and somatic cells in relation to milking technology. J. Agrobiol., 28, 1: 49-54. ISSN 1803-4403. DOI: 10.2478/v10146-011-0005-8 Go to original source...
    35. O'BRIAN, B., O'CALLAGHAN, E., DILLON, P., 1998: Effect of milking machine systems and components on free fatty acid levels in milk. J. Dairy Res., 65: 335-339. ISSN 1469-7629. Go to original source...
    36. PETERKOVÁ, L., 2002: Free fatty acids ratio in milk, factors which affect their concentration and possibilities their determination. (In Czech) Problematika prvovýroby mléka XXVI, Medlov, Milcom a. s., Praha, 26-30.
    37. SANTOS, M. V., MA, Y., BARBANO, D. M., 2003: Effect of somatic cell count on proteolysis and lipolysis in pasteurized fluid milk during shelf-life storage. J. Dairy Sci., 86: 2491-2503. ISSN 0022-0302. DOI: 10.3168/jds.S0022-0302(03)73843-0 Go to original source...
    38. THOMSON, N. A., WOOLFORD, W. M., COPEMAN, A. P. J., 2005: Milk harvesting and cow factors influencing seasonal variation in the levels of free fatty acids in milk from Waikato dairy herds. New Zeal. J. Agr. Res., 48: 11-21. ISSN 0028-8233. DOI: 10.1080/00288233.2005.9513626 Go to original source...
    39. TORKAR, K. G., TEGER, S. G., 2008: The microbiological quality of raw milk after introducing the two day's milk collecting system. Acta Agric. Slov., 92: 61-74. ISSN 1854-4800.
    40. SHELLEY, A. W., DEETH, H. C., MACRAE, I. C., 1987: A numerical taxonomic study of psychrotrophic bacteria associated with lipolytic spoilage of raw milk. J. Appl. Bacteriol., 62: 197-207. ISSN 0021-8847. DOI: 10.1111/j.1365-2672.1987.tb02399.x Go to original source...
    41. SJAUNJA, L. O., 1984: Studies on milk analysis of individual cow milk samples. III. The effect of different treatments on infrared analyses. Acta Agric. Scand., 34: 273-285. ISSN 0906-4710. DOI: 10.1080/00015128409435396 Go to original source...
    42. SOJKOVÁ, K., HANUŠ, O., KOPECKÝ, J., JEDELSKÁ, R., 2009: Determination of thermogradient for interlaboratory milk sample transport. (In Czech) Výzkum v chovu skotu / Cattle Research, LI, 187, 3: 35-41. ISSN 0139-7265.
    43. VYLETĚLOVÁ, M., BENDA, P., HANUŠ, O., KOPUNECZ, P., 1999 a: Determination of total psychrotrophic microorganisms in bulk milk samples and their relationship to total count of mikroorganisms. (In Czech) Czech J. Food Sci., 17, 6: 216-222. ISSN 1212-1800.
    44. VYLETĚLOVÁ, M., FICNAR, J., HANUŠ, O., 2000 a: Effects of lipolytic enzymes Pseudomonas fluorescens on liberation of fatty acids from milk fat. Czech J. Food Sci., 18, 5: 175-182. ISSN 1212-1800. DOI: 10.17221/8339-CJFS Go to original source...
    45. VYLETĚLOVÁ, M., HANUŠ, O., URBANOVÁ, E., 1999 b: The occurrence of proteolytical and lipolytical bacteria in cow bulk milk samples. (In Czech) Veterinářství, 49, 11: 480-482. ISSN 0506-8231.
    46. VYLETĚLOVÁ, M., HANUŠ, O., URBANOVÁ, E., KOPUNECZ, P., 2000 b: The occurrence and identification of psychrotrophic bacteria with proteolytic and lipolytic activity in bulk milk samples at storage in primary production conditions. (In Czech) Czech J. Anim. Sci., 45: 373-383. ISSN 1212-1819.
    47. WIKING, L., NIELSEN, J. H., BAVIUS, A. K., EDVARDSSON, A., SVENNERSTEN-SJAUNJA, K., 2006: Impact of milking frequencies on the level of free fatty acids in milk, fat globule size, and fatty acid composition. J. Dairy Sci., 89: 1004-1009. ISSN 0022-0302. DOI: 10.3168/jds.S0022-0302(06)72166-X Go to original source...
    48. WIKING, L., BJÖRCK, L., NIELSEN, J. H., 2003: Influence of feed composition on stability of fat globules during pumping of raw milk. Inter. Dairy J., 13: 797-803. ISSN 0958-6946. DOI: 10.1016/S0958-6946(03)00110-9 Go to original source...

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