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<article article-type="research-article" dtd-version="1.3" xmlns:mml="http://www.w3.org/1998/Math/MathML" xmlns:xlink="http://www.w3.org/1999/xlink" xmlns:xsi="http://www.w3.org/2001/XMLSchema-instance" xml:lang="ru"><front><journal-meta><journal-id journal-id-type="publisher-id">rmjournal</journal-id><journal-title-group><journal-title xml:lang="ru">Эталоны. Стандартные  образцы</journal-title><trans-title-group xml:lang="en"><trans-title>Measurement Standards. Reference Materials</trans-title></trans-title-group></journal-title-group><issn pub-type="ppub">2687-0886</issn><publisher><publisher-name>D. I. Mendeleyev Institute for Metrology</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="doi">10.20915/2077-1177-2024-20-4-57-75</article-id><article-id custom-type="elpub" pub-id-type="custom">rmjournal-520</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Article</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="ru"><subject>Современные методы анализа веществ и материалов</subject></subj-group><subj-group subj-group-type="section-heading" xml:lang="en"><subject>Modern methods of analysis of substances and materials</subject></subj-group></article-categories><title-group><article-title>Совершенствование   Государственной первичной референтной методики измерений массовой доли жира в пищевых продуктах и продовольственном сырье</article-title><trans-title-group xml:lang="en"><trans-title>Improvement of the State Primary Reference Measurement Procedure for the Determination of Mass Fraction of Fat Content in Food Products and Food Raw Materials</trans-title></trans-title-group></title-group><contrib-group><contrib contrib-type="author" corresp="yes"><contrib-id contrib-id-type="orcid">https://orcid.org/0000-0001-8347-2633</contrib-id><name-alternatives><name name-style="eastern" xml:lang="ru"><surname>Сергеева</surname><given-names>А. С.</given-names></name><name name-style="western" xml:lang="en"><surname>Sergeeva</surname><given-names>A. S.</given-names></name></name-alternatives><bio xml:lang="ru"><p>Сергеева Анна Сергеевна – канд. хим. наук, старший научный сотрудник лаборатории метрологии влагометрии и стандартных образцов</p><p>Researcher ID: AAE-7942–2021</p><p>620075,  г. Екатеринбург, ул. Красноармейская, д.4 </p><p> </p></bio><bio xml:lang="en"><p>Anna S. Sergeeva – Cand. Sci. (Chem.), Senior Researcher of the Laboratory for Metrological Support of Moisture Measurement and Reference Materials</p><p>Researcher ID: AAE-7942–2021</p><p> 4 Krasnoarmeyskaya st., Yekaterinburg, 620075</p></bio><email xlink:type="simple">sergeevaas@uniim.ru</email><xref ref-type="aff" rid="aff-1"/></contrib></contrib-group><aff-alternatives id="aff-1"><aff xml:lang="ru"><institution>Уральский научно-исследовательский институт метрологии – филиал ФГУП «ВНИИМ им. Д. И. Менделеева»</institution><country>Россия</country></aff><aff xml:lang="en"><institution>UNIIM – Affiliated Branch of the D. I. Mendeleyev Institute for Metrology</institution><country>Russian Federation</country></aff></aff-alternatives><pub-date pub-type="collection"><year>2024</year></pub-date><pub-date pub-type="epub"><day>04</day><month>01</month><year>2025</year></pub-date><volume>20</volume><issue>4</issue><fpage>57</fpage><lpage>75</lpage><permissions><copyright-statement>Copyright &amp;#x00A9; Сергеева А.С., 2024</copyright-statement><copyright-year>2024</copyright-year><copyright-holder xml:lang="ru">Сергеева А.С.</copyright-holder><copyright-holder xml:lang="en">Sergeeva A.S.</copyright-holder><license xml:lang="ru" license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>Данная работа распространяется под лицензией Creative Commons Attribution 4.0.</license-p></license><license xml:lang="en" license-type="creative-commons-attribution" xlink:href="https://creativecommons.org/licenses/by/4.0/" xlink:type="simple"><license-p>This work is licensed under a Creative Commons Attribution 4.0 License.</license-p></license></permissions><self-uri xlink:href="https://www.rmjournal.ru/jour/article/view/520">https://www.rmjournal.ru/jour/article/view/520</self-uri><abstract><p>С целью обеспечения метрологической прослеживаемости измерений массовой доли жира в 2018 году была разработана, аттестована и утверждена Государственная первичная референтная методика измерений массовой доли жира в пищевых продуктах и продовольственном сырье (ГПРМИ). ГПРМИ распространяется на пробы молока сухого, сметаны, творога, сыра, мяса и мясных продуктов, сухих яичных продуктов, смеси молочной, каши зерновой, зерно-молочной, консервов для детского питания и устанавливает требования к процедуре измерений массовой доли жира экстракционно-гравиметрическим методом Рэнделла. В процессе применения ГПРМИ была выявлена необходимость расширения области ее применения.</p><p>Цель представленного в статье исследования – совершенствование ГПРМИ массовой доли жира в пищевых продуктах и продовольственном сырье. По ходу исследования выполнен анализ нормативных документов, определяющих требования к новым объектам измерений, диапазонам измерений и показателям точности. Установлены параметры измерений и их допускаемые пределы варьирования для новых объектов.</p><p>В результате совершенствования в область применения ГПРМИ включены молоко и сливки питьевые, молоко и сливки сгущенные, филе рыбное, мясо рыбы, включая фарш, хлебобулочные изделия, мучные кондитерские изделия, макаронные изделия, какао-порошок, шоколад, мука из зерновых культур, орехов, паста ореховая, в т. ч. арахисовая. Оценка показателей точности ГПРМИ проведена с использованием стандартных образцов утвержденного типа, пищевых продуктов и продовольственного сырья.</p><p>Разработанная процедура измерений обеспечивает запас по точности результатов измерений по ГПРМИ в сравнении со стандартизованными методиками измерений от двух до 25 раз в зависимости от объекта и диапазона измерений. В рамках проведения межлабораторных сличительных испытаний опробована процедура применения ГПРМИ для оценки правильности результатов измерений, полученных с использованием стандартизованных методик измерений.</p><p>В ходе проведения пилотных сличений КООМЕТ, а также анализа зарубежных стандартных образцов продемонстрирована эквивалентность ГПРМИ аналогичным методикам измерений иностранных государств. Показана применимость ГПРМИ для определения аттестованного значения массовой доли жира при характеризации стандартных образцов.</p></abstract><trans-abstract xml:lang="en"><p>In order to ensure metrological traceability of fat mass fraction measurements, the State Primary Reference Measurement Procedure (SPRMP) for the Determination of Mass Fraction of Fat in Food Products and Food Raw Materials was developed, certified and approved in 2018. The SPRMP applies to samples of milk powder, sour cream, cottage cheese, cheese, meat and meat products, dry egg products, milk mixtures, grain porridge, grain-milk mixtures, canned baby food and establishes requirements for the procedure for measuring the mass fraction of fat using the Randall extractiongravimetric method. In the process of applying the SPRMP, the need to expand the scope of its application was identified. The purpose of the research is to improve the SPRMP of the mass fraction of fat in food products and food raw materials. An analysis of regulatory documents defining requirements for new measurement objects, measurement ranges and accuracy indicators has been completed. The measurement parameters and their permissible variation limits for new objects have been established. As a result of improvement, the scope of application of the SPRMP includes drinking milk and cream, condensed milk and cream, fish fillet, fish meat, including minced meat, bakery products, f lour confectionery, pasta, cocoa powder, chocolate, flour from cereals, nuts, nut paste, including peanut. An assessment of the accuracy indicators of the SPRMP was carried out using certified reference materials, food products and food raw materials. The developed measurement procedure made it possible to ensure a margin of accuracy of the measurement results using the SPRMP in comparison with standardized measurement procedures from 2 to 25 times, depending on the object and the measurement range. As part of the interlaboratory comparison tests, the procedure for using the SPRMP to assess the correctness of measurement results obtained using standardized measurement procedures was tested. During the COOMET pilot comparisons, as well as the analysis of foreign reference materials, the equivalence of the SPRMP to similar measurement methods of foreign countries was demonstrated. The applicability of the SPRMP for determining the certified value of the mass fraction of fat during the characterization of reference materials was demonstrated.</p></trans-abstract><kwd-group xml:lang="ru"><kwd>метрологическая прослеживаемость</kwd><kwd>первичная референтная методика измерений</kwd><kwd>массовая доля жира</kwd><kwd>метод Рэнделла</kwd><kwd>пищевые продукты</kwd></kwd-group><kwd-group xml:lang="en"><kwd>metrological traceability</kwd><kwd>primary reference measurement procedure</kwd><kwd>mass fraction of fat</kwd><kwd>Randall method</kwd><kwd>food products</kwd></kwd-group><funding-group><funding-statement xml:lang="ru">Работа выполнена в рамках внутренней НИР «Пищевая ценность» (рег. номер ИКРБС 123081600025–4 от 16.08.2023)</funding-statement><funding-statement xml:lang="en">The work was carried out within the framework of the internal research project «Food value» (reg. number IKRBS123081600025–4 dated 16.08.2023).</funding-statement></funding-group></article-meta></front><back><ref-list><title>References</title><ref id="cit1"><label>1</label><citation-alternatives><mixed-citation xml:lang="ru">Reference measurement procedure for the determination of mass fraction of fat content in food / S. V. Medvedevskikh [et al.] // Accreditation and Quality Assurance. 2021. Vol. 26. P. 165–175. https://doi.org/10.1007/s00769-021-01472-w</mixed-citation><mixed-citation xml:lang="en">Medvedevskikh S. V., Baranovskaya V. B., Medvedevskikh M. Yu., Krasheninina M. P., Sergeeva A. S. Reference measurement procedure for the determination of mass fraction of fat content in food. Accreditation and Quality Assurance. 2021;26:165–175. https://doi.org/10.1007/s00769-021-01472-w</mixed-citation></citation-alternatives></ref><ref id="cit2"><label>2</label><citation-alternatives><mixed-citation xml:lang="ru">Применение первичных референтных методик измерений в сфере обеспечения единства измерений / А. С. Сергеева [и др.] // Законодательная и прикладная метрология. 2020. № 5 (167). С. 5–9.</mixed-citation><mixed-citation xml:lang="en">Sergeeva A. S., Medvedevskikh M. Yu., Studenok V. V., Parfenova E. G. Use of primary reference measurement techniques in the field of assurance of measurement uniformity. Legal and applied metrology. 2020;5(167):5–9. (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit3"><label>3</label><citation-alternatives><mixed-citation xml:lang="ru">Первичные референтные методики измерений в пищевой промышленности: опыт применения и перспективы развития / А. С. Сергеева [и др.] // Эталоны. Стандартные образцы. 2023. Т. 19, № 4. С. 83–98. https://doi.org/10.20915/2077-1177-2023-19-4-83-98</mixed-citation><mixed-citation xml:lang="en">Sergeeva A. S., Kasilyunas A. V., Parfenova E. G., Medvedevskikh S. V. Primary reference measurement procedures in the food industry: usage experience and development prospects. Measurement standards. Reference materials. 2023;19(4):83–98. (In Russ.). https://doi.org/10.20915/2077-1177-2023-19-4-83-98</mixed-citation></citation-alternatives></ref><ref id="cit4"><label>4</label><citation-alternatives><mixed-citation xml:lang="ru">Сергеева А. С. Актуальные вопросы определения содержания жира в пищевых продуктах и продовольственном сырье (обзор) // Эталоны. Стандартные образцы. 2024. Т. 20, № 1. С. 59–84. https://doi.org/10.20915/2077-1177-2024-20-1-59-84</mixed-citation><mixed-citation xml:lang="en">Sergeeva A. S. Current Issues in determining fat content in food products and food raw materials (Review). Measurement Standards. Reference Materials. 2024;20(1):59–84. (In Russ.). https://doi.org/10.20915/2077-1177-2024-20-1-59-84</mixed-citation></citation-alternatives></ref><ref id="cit5"><label>5</label><citation-alternatives><mixed-citation xml:lang="ru">Randall E. L. Improved method for fat and oil analysis by a new process of extraction // Journal of Association of Official Analytical Chemists. 1974. Vol. 57, № 5. P. 1165–1168. https://doi.org/10.1093/jaoac/57.5.1165</mixed-citation><mixed-citation xml:lang="en">Randall E. L. Improved method for fat and oil analysis by a new process of extraction. Journal of Association of Official Analytical Chemists. 1974;57(5):1165–1168. https://doi.org/10.1093/jaoac/57.5.1165</mixed-citation></citation-alternatives></ref><ref id="cit6"><label>6</label><citation-alternatives><mixed-citation xml:lang="ru">Shin J.-M., Park S.-K. Comparison of fat determination methods depending on fat definition in bakery products // LWT – Food Science and Technology. 2015. Vol. 63, № 2. P. 972–977. https://doi.org/10.1016/j.lwt.2015.04.011</mixed-citation><mixed-citation xml:lang="en">Shin J.-M., Park S.-K. Comparison of fat determination methods depending on fat definition in bakery products. LWT Food Science and Technology. 2015;63(2):972–977. https://doi.org/10.1016/j.lwt.2015.04.011</mixed-citation></citation-alternatives></ref><ref id="cit7"><label>7</label><citation-alternatives><mixed-citation xml:lang="ru">Zhang Y., Zhao J., Yang H.-W. Comparison and analysis of goodness of fit and fitting formula between milk fat concentration and refractive index // International Journal of Modeling, Simulation, and Scientific Computing. 2024. Vol. 15, № 3. P. 2450022. https://doi.org/10.1142/S1793962324500223</mixed-citation><mixed-citation xml:lang="en">Zhang Y., Zhao J., Yang H.-W. Comparison and analysis of goodness of fit and fitting formula between milk fat concentration and refractive index. International Journal of Modeling, Simulation, and Scientific Computing. 2024;15(03):2450022. https://doi.org/10.1142/S1793962324500223</mixed-citation></citation-alternatives></ref><ref id="cit8"><label>8</label><citation-alternatives><mixed-citation xml:lang="ru">Desai P., Pandya U. Optical Butyrometric reading tube: An approach towards Gerber automation // Indian Journal of Dairy Science. 2022. Vol. 75, № 6. P. 536–541. https://doi.org/10.33785/IJDS.2022.v75i06.007</mixed-citation><mixed-citation xml:lang="en">Desai P., Pandya U. Optical Butyrometric reading tube: An approach towards Gerber automation. Indian Journal of Dairy Science. 2022;75(6):536–541. https://doi.org/10.33785/IJDS.2022.v75i06.007</mixed-citation></citation-alternatives></ref><ref id="cit9"><label>9</label><citation-alternatives><mixed-citation xml:lang="ru">Wu D., Feng S., He Y. Infrared Spectroscopy Technique for the Nondestructive Measurement of Fat Content in Milk Powder // Journal of Dairy Science. 2007. Vol. 90, № 8. P. 3613–3619. https://doi.org/10.3168/jds.2007-0164</mixed-citation><mixed-citation xml:lang="en">Wu D., Feng S., He Y. Infrared Spectroscopy Technique for the Nondestructive Measurement of Fat Content in Milk Powder. Journal of Dairy Science. 2007;90(8):3613–3619. https://doi.org/10.3168/jds.2007-0164</mixed-citation></citation-alternatives></ref><ref id="cit10"><label>10</label><citation-alternatives><mixed-citation xml:lang="ru">NIRS and MIRS technique for the determination of protein and fat content in milk powder / D. Wu [et al.] // Proc. SPIE6625, International Symposium on Photoelectronic Detection and Imaging 2007: Related Technologies and Applications. 2008. 66251S. https://doi.org/10.1117/12.791230</mixed-citation><mixed-citation xml:lang="en">Wu D., Feng S., He C., He Y. NIRS and MIRS technique for the determination of protein and fat content in milk powder. Proc. SPIE6625, International Symposium on Photoelectronic Detection and Imaging 2007: Related Technologies and Applications. 2008:66251S. https://doi.org/10.1117/12.791230</mixed-citation></citation-alternatives></ref><ref id="cit11"><label>11</label><citation-alternatives><mixed-citation xml:lang="ru">Ultrasound velocity to measure beef, chicken and fish fillet fat content / M. H. A. Halim [et al.] // 2012 IEEE Student Conference on Research and Development (SCOReD), Pulau Pinang, Malaysia, 2012. P. 54–58. https://doi.org/10.1109/SCOReD.2012.6518610</mixed-citation><mixed-citation xml:lang="en">Halim M. H. A., Buniyamin N., Shari M. A. M., Kassim R. A. Ultrasound velocity to measure beef, chicken and fish fillet fat content. 2012 IEEE Student Conference on Research and Development (SCOReD), Pulau Pinang, Malaysia. 2012:54–58. https://doi.org/10.1109/SCOReD.2012.6518610</mixed-citation></citation-alternatives></ref><ref id="cit12"><label>12</label><citation-alternatives><mixed-citation xml:lang="ru">Leung H. K., Anderson G. R., Norr P. J. Rapid Determination of Total and Solid Fat Contents in Chocolate Products by Pulsed Nuclear Magnetic Resonance // Journal of Food Science. 1985. Vol. 50, № 4. P. 942–945. https://doi.org/ 10.1111/j.1365-2621.1985.tb12985.x</mixed-citation><mixed-citation xml:lang="en">Leung H. K., Anderson G. R., Norr P. J. Rapid Determination of Total and Solid Fat Contents in Chocolate Products by Pulsed Nuclear Magnetic Resonance. Journal of Food Science. 1985;50(4):942–945. https://doi.org/10.1111/j.1365-2621.1985.tb12985.x</mixed-citation></citation-alternatives></ref><ref id="cit13"><label>13</label><citation-alternatives><mixed-citation xml:lang="ru">Дерффель К. Статистика в аналитической химии. Пер. с нем. М. : Мир, 1994. 268 с.</mixed-citation><mixed-citation xml:lang="en">Doerffel V. K. Statistik in der analytischen Chemie. Moscow: Mir; 1994. 268 p. (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit14"><label>14</label><citation-alternatives><mixed-citation xml:lang="ru">Сергеева А. С., Касилюнас А. В., Голынец О. С. О ходе разработки стандартных образцов состава шоколада // Альманах современной метрологии. 2024. № 2 (38). С. 65–77.</mixed-citation><mixed-citation xml:lang="en">Sergeeva A. S., Kasilyunas A. V., Golynets O. S. The progress of development of certified reference material for composition of chocolate. Al’manac of Modern Metrology. 2024;2(38):65–77. (In Russ.).</mixed-citation></citation-alternatives></ref><ref id="cit15"><label>15</label><citation-alternatives><mixed-citation xml:lang="ru">Сергеева А. С., Первухина О. Е., Голынец О. С. О ходе разработки стандартного образца состава муки миндальной // Метрология 2024 : Материалы международной научно-технической конференции, Минск, 9–10 апреля 2024 года. Минск : БелГИМ, 2024. С. 255–259.</mixed-citation><mixed-citation xml:lang="en">Sergeeva A. S., Pervukhina O. E., Golynets O. S. The progress of development of certified reference material for composition of almond flour. Metrology 2024. Materials of the international scientific and technical conference, Minsk, 9–10 April 2024. Minsk: BelGIM; 2024. 255–259 p. (In Russ.).</mixed-citation></citation-alternatives></ref></ref-list><fn-group><fn fn-type="conflict"><p>The authors declare that there are no conflicts of interest present.</p></fn></fn-group></back></article>
