Application of the lyophilization system for preparation of reference materials for composition of nutrition products

The article presents the application of the lyophilization system for preparation of reference materials (RM) for composition of nutritive products samples. The purpose of the research was the development of lyophilization procedure of RM for composition of poultry meat samples preparation with certified values of mass fraction of moisture, nitrogen (protein) and fat.

The poultry meat of two types was used as the primary material for RM for poultry meat composition preparation -1) white meat (chicken breast); 2) red meat (chicken thigh). The procedure included pounding, boiling, freezing and lyophilisation (syn. freeze drying). The researches for homogeneity were implemented with hot air dryer standard system from the State primary standard GET 173-2017. Measurement of nitrogen (protein) mass fraction was performed on State secondary standard GVET176-1-2010. Measurements of fat mass fraction were performed with accordance to State Primary Reference Measurement Procedure.

The total time of lyophilization process for samples № 1 and № 2 was 19 and 28 hours, respectively. The total mass loss for sample № 1 was about 63 %, for sample № 2 was about 65 %. The difference in material moisture mass fraction values of materials dried on different trays of freeze dryer was statistically significant, i. e., material was non-homogeneous. To obtain a homogeneous material, an additional homogenization procedure was performed: grinding in a laboratory mill, sieving through a sieve, thorough mixing and conditioning. The certified values of moisture, nitrogen, protein, fat mass fraction for the sample № 1 were accordingly 4,5 %, 14,74 %, 92,1 %, 7,9 %. The same values in the same sequence were 6,3 %, 12,21 %, 76,3 %, 23,8 %.

The procedure of lyophilisation was developed for production of reference materials for composition of boiled and freeze-dried poultry meat. The usage of this lyophilisation system allowed to ensure a RM expiration date of six months at ambient temperature of (7±3) °C and relative humidity no more than 60 %. The Reference Materials for composition of boiled and freeze-dried poultry meat was added into Register of certified RMs under № GSO 11276-2019 by the results.

1. ISO Guide 35:2017 Reference materials - Guidance for characterization and assessment of homogeneity and stability. Geneve: ISO; 2017.

2. Panfilov V. A. Theoretical foundations of food technologies. In 2 books. Of book 2. Moscow: Kolos; 2009. 800 p. (In Russ.).

3. Ooghe W., Kramer G. N., Schimmel H., Pauwels J. Comparison of some additives used in the preparation of freeze-dried lemon juice candidate reference materials. Fresenius journal of analytical chemistry. 1998;360(3-4):445-448. https://doi.org/10.1007/s002160050734.

4. Kramer G. N., Angelis L. D., Pauwels J., Ooghe W., Belliardo J. J. The freeze-drying of orange juice for the preparation of reference materials. Fresenius journal of analytical chemistry. 1988;332: 694-697. https://doi.org/10.1007/BF00472671.

5. Ihnat M., Cloutier R., Wood D. Reference materials for agricultural and food analysis: preparation and physical characterization of a bovine muscle powder candidate reference material. Fresenius' zeitschrift fur analytische chemie. 1987;326:627-633. https://doi.org/10.1007/BF00473517.

6. Bertolin J. R., Joy M., Rufino-Moya P. J., Lobon S., Blanco M. Simultaneous determination of carotenoids, tocopherols, retinol and cholesterol in ovine lyophilised samples of milk, meat, and liver and in unprocessed raw samples of fat. Food Chemistry. 2018;257:182-188. https://doi.org/10.1016/j.foodchem.2018.02.139.

7. Carron P., Emteborg H., Hess P. Freeze-drying for the stabilisation of shellfish toxins in mussel tissue (Mytilus edulis) reference materials. Analytical and bioanalytical chemistry. 2007;387(7):2475-2486. https://doi.org/10.1007/s00216-006-1104-z.

8. Josephs R., Ulberth F. E., Van Egmond H. P, Emons H. Aflatoxin M1 in milk powders: Processing, homogeneity and stability testing of certified reference materials. Food Additives and Contaminants. 2005;22(9):864-874. https://doi.org/10.1080/0265203050016653.

9. Huertas-Perez J. F., Bordajandi L. R., Sejeroe-Olsen B., Emteborg H., Bail A., Schimmel H., Dabrio M. Pahs in baby food: assessment of three different processing techniques for the preparation of reference materials. Analytical and bioanalytical chemistry. 2015;407:3069-3081. https://doi.org/10.1007/s00216-015-8490-z.

10. Saldanha H., Olsen S. B., Ulberth F., Emons H., Zeleny R., Grimalt S. Development of a new cucumber reference material for pesticide residue analysis: feasibility study for material processing, homogeneity and stability assessment. Analytical and bioanalytical chemistry. 2015;407:3083-3091. https://doi.org/10.1007/s00216-015-8476-x.

11. Zeleny R., Emteborg H., Charoud-Got J., Schimmel H., Nia Y., Mutel I., Ostyn A., Herbin S., Hennekinne J.-A. Development of a reference material for staphylococcus aureus enterotoxin А in cheese: feasibility study, processing, homogeneity and stability assessment. Food chemistry. 2015;168:241-246. https://doi.org/10.1016/j.foodchem.2014.07.066.

12. Won S. H., Lee С-H., Kim B. Development of certified reference materials for accurate determination of fluoroquinolone antibiotics in chicken meat. Food Chemistry. 2017;229:472-478. https://doi.org/10.1016/j.foodchem.2017.02.112.

13. Medvedevskikh M. Y., Sergeeva A. S., Krasheninina M. P., Shokhina O. S. Creating reference standards for the implementation of the State verification scheme for water content measurement. Measurement Techniques. 2019;62(6):475-483. (In Russ). https://doi.org/10.1007/s11018-019-01649-3.

14. Krasheninina M. P., Medvedevskikh M. Yu., Medvedevskikh S. V., Sobina E. P., Neudachina L. K. An estimate of the metrological characteristics of a standard sample of the composition of dried whole milk using primary and secondary state standards. Measurement Techniques. 2013;56(9):1076-1082. (In Russ). https://doi.org/10.1007/s11018-013-0333-8.

15. Ivanov V. P., Medvedevskikh S. V. Processing of the measurement results of water content in solid substances. Guidelines. Sverdlovsk: Uro AN SSSR; 1988. 200 p. (In Russ).

16. Bol'shev L. N., Smirnov N. V. Tables of mathematical statistics. Moscow: Science. Main editorial office of physical and mathematical literature; 1983. 416 p. (In Russ).

17. Medvedevskikh M. Yu., Sergeeva A. S., Krasheninina M. P., Vostrikova N. L., Semenova A. A., Kuznetsova O. A. About the development of reference materials of meat and meat product composition. Journal of physics: conference series. 2019;1420:012030. https://doi.org/10.1088/1742-6596/1420/1/012030.