litosphereЛитосфераLITHOSPHERE (Russia)1681-90042500-302XA.N. Zavaritsky Institute of Geology and Geochemistry10.24930/1681-9004-2025-25-2-355-364WIOQMElitosphere-2282Research ArticleСИНТЕЗ И СВОЙСТВА МИНЕРАЛОПОДОБНЫХ МАТЕРИАЛОВSYNTHESIS AND PROPERTIES OF MINERAL-LIKE MATERIALSИнжектируемые костные цементы на основе магний-замещенного витлокита, содержащие натрий карбокисметиллцеллюлозуInjected bone cements based on magnesium-substituted whitlockite, containing sodium carboxymethyl celluloseГольдбергМ. А.GoldbergM. A.

119334; Ленинский пр-т, 49; Москва

Margarita A. Goldberg

119334; 49 Leninsky av.; Moscow

mgoldberg@imet.ac.ruКрохичеваП. А.KrokhichevaP. A.

119334; Ленинский пр-т, 49; Москва

Polina A. Krokhicheva

119334; 49 Leninsky av.; Moscow

ХайрутдиноваД. Р.KhayrutdinovaD. R.

119334; Ленинский пр-т, 49; Москва

Dinara R. Khayrutdinova

119334; 49 Leninsky av.; Moscow

ФоминА. С.FominA. S.

119334; Ленинский пр-т, 49; Москва

Aleksander S. Fomin

119334; 49 Leninsky av.; Moscow

ЛеоновА. В.LeonovA. V.

119991; Ленинские горы, 1A; Москва

Aleksander V. Leonov

119991; 1А Lenin Hills; Moscow

БаикинА. С.BaikinA. S.

119334; Ленинский пр-т, 49; Москва

Aleksander S. Baikin

119334; 49 Leninsky av.; Moscow

АнтоноваО. С.AntonovaO. S.

119334; Ленинский пр-т, 49; Москва

Olga S. Antonova

119334; 49 Leninsky av.; Moscow

СенцоваА. М.SentsovaA. M.

119334; Ленинский пр-т, 49; Москва

Anita M. Sentsova

119334; 49 Leninsky av.; Moscow

ДонскаяН. О.DonskayaN. O.

119334; Ленинский пр-т, 49; Москва

Nadezhda O. Donskaya

119334; 49 Leninsky av.; Moscow

БариновС. М.BarinovS. M.

119334; Ленинский пр-т, 49; Москва

Sergey M. Barinov

119334; 49 Leninsky av.; Moscow

КомлевВ. С.KomlevV. S.

119334; Ленинский пр-т, 49; Москва

Vladimir S. Komlev

119334; 49 Leninsky av.; Moscow

Институт металлургии и материаловедения им. А.А. Байкова РАНРоссияA.A. Baikov Institute of Metallurgy and Materials Science, RASRussian FederationМосковский государственный университет имени М.В. ЛомоносоваРоссияM.V. Lomonosov Moscow State University, 1А Lenin HillsRussian Federation202504052025252Минералы: строение, свойства, методы исследования355364Copyright © Гольдберг М.А., Крохичева П.А., Хайрутдинова Д.Р., Фомин А.С., Леонов А.В., Баикин А.С., Антонова О.С., Сенцова А.М., Донская Н.О., Баринов С.М., Комлев В.С., 20252025Гольдберг М.А., Крохичева П.А., Хайрутдинова Д.Р., Фомин А.С., Леонов А.В., Баикин А.С., Антонова О.С., Сенцова А.М., Донская Н.О., Баринов С.М., Комлев В.С.Goldberg M.A., Krokhicheva P.A., Khayrutdinova D.R., Fomin A.S., Leonov A.V., Baikin A.S., Antonova O.S., Sentsova A.M., Donskaya N.O., Barinov S.M., Komlev V.S.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://www.lithosphere.ru/jour/article/view/2282   Объект исследования

   Объект исследования. Кальций-магний фосфатные порошки и цементные материалы, а также цементная жидкость, содержащая натрий карбоксил метилцеллюлозу (КМЦ).

   Цель

   Цель. Создание инжектируемых костных цементов на основе растворимых фаз фосфатов кальция и магния для потенциального применения в малоинвазивных хирургических вмешательствах.

   Методы

   Методы. Для характеристики материалов использовали лазерный анализатор частиц Fritsch Analysis 22, дифрактометр Shimadzu XRD-6000, растровый электронный микроскоп Tescan Vega II с установкой для энергодисперсионного анализа Inca X-Act Oxford Instruments, анализатор частиц Tristar 3000, вискозиметр Brookfield DV2T, универсальные испытательные машины Instron 5581 и Instron 3382.

   Результаты

   Результаты. Благодаря введению КМЦ был достигнут рост вязкости и поверхностного натяжения цементной жидкости, что обеспечило улучшение характеристик инжектируемости и когезии в водной среде полученных цементных материалов. Было установлено влияние механоактивации цементных порошков, а также введения КМЦ в цементную жидкость на фазовый состав, время схватывания цементов, их микроструктуру, когезию, инжектируемость и прочностныесвойства.

   Research subject

   Research subject. Calcium-magnesium phosphate powder and cement materials and cement fluid containing sodium carboxymethylcellulose (CMC).

   Aim

   Aim. To develop injectable bone cements based on soluble phases of calcium and magnesium phosphates for possible use in minimally invasive surgery.

   Methods

   Methods. Fritsch Analysis 22 laser particle analyser, Shimadzu XRD-6000 diffractometer, Tescan Vega II scanning electron microscope with an Oxford Instruments Inca X-Act energy dispersive analyser, Tristar 3000 particle analyser, Brookfield DV2T viscometer, Instron 5581 and Instron 3382 universal testing machines were used to characterise the materials.

   Results

   Results. The introduction of CMC resulted in an increase in the viscosity and surface tension of the cement fluid, which resulted in an increase in the injectability and cohesion in aqueous media of the resulting cement materials. The effects of CMC introduction and mechanochemical activation on the phase composition, setting time, microstructure, cohesion, injectability and strength properties of the cement materials were determined.

костные цементыфосфат кальцияфосфат магниякарбоксиметилцеллюлозаинжектируемостькогезиямагний-замещенный витлокитгидроксиапатитbone cementscalcium phosphatemagnesium phosphatecarboxymethylcelluloseinjectabilitycohesionmagnesium-substituted whitlockitehydroxyapatiteРабота выполнена в рамках государственного задания ИМЕТ РАН № 075-00319-25-00The work was carried out with the support of A.A. Baikov Institute of Metallurgy and Materials Science, Russian Academy of Sciences State assignment No. 075-00319-25-00ReferencesBarth J.A., Verbeeck R.M.H. (1984) The CaO-MgO-P,O, System Das Ca0-Mg0-P206-8ystem boi 1000°C fur P z O ~ <33,3 Mo1-X. Z. anorg. allg. Chem., 515.Barth J.A., Verbeeck R.M.H. (1984) The CaO-MgO-P,O, System Das Ca0-Mg0-P206-8ystem boi 1000°C fur P z O ~ <33,3 Mo1-X. Z. anorg. allg. Chem., 515.Cahyanto A., Imaniyyah A.G., Zakaria M.N., Hasratiningsih Z. (2017) Mechanical Strength Properties of Injectable Carbonate Apatite Cement with Various Concentration of Sodium Carboxymethyl Cellulose. Key Engin. Mater., 758, 56-60. doi: 10.4028/WWW.SCI-ENTIFIC.NET/KEM.758.56Cahyanto A., Imaniyyah A.G., Zakaria M.N., Hasratiningsih Z. (2017) Mechanical Strength Properties of Injectable Carbonate Apatite Cement with Various Concentration of Sodium Carboxymethyl Cellulose. Key Engin. Mater., 758, 56-60. doi: 10.4028/WWW.SCI-ENTIFIC.NET/KEM.758.56Demir-Oğuz Ö., Boccaccini A.R., Loca D. (2023) Injectable bone cements: What benefits the combination of calcium phosphates and bioactive glasses could bring? Bioactive Mater., 19, 217-236. doi: 10.1016/J.BIOACT-MAT.2022.04.007Demir-Oğuz Ö., Boccaccini A.R., Loca D. (2023) Injectable bone cements: What benefits the combination of calcium phosphates and bioactive glasses could bring? Bioactive Mater., 19, 217-236. doi: 10.1016/J.BIOACT-MAT.2022.04.007Goldberg M.A., Krohicheva P.A., Fomin A.S., Khairutdinova D.R., Antonova O.S., Baikin A.S., Smirnov V.V., Fomina A.A., Leonov A.V., Mikheev I.V., Sergeeva N.S., Akhmedova S.A., Barinov S.M., Komlev V.S. (2020a) Insitu magnesium calcium phosphate cements formation: From one pot powders precursors synthesis to in vitro investigations. Bioactive Mater., 5(3), 644-658. doi: 10.1016/j.bioactmat.2020.03.011Goldberg M.A., Krohicheva P.A., Fomin A.S., Khairutdinova D.R., Antonova O.S., Baikin A.S., Smirnov V.V., Fomina A.A., Leonov A.V., Mikheev I.V., Sergeeva N.S., Akhmedova S.A., Barinov S.M., Komlev V.S. (2020a) Insitu magnesium calcium phosphate cements formation: From one pot powders precursors synthesis to in vitro investigations. Bioactive Mater., 5(3), 644-658. doi: 10.1016/j.bioactmat.2020.03.011Jacquart S., Girod-Fullana S., Brouillet F., Pigasse C., Siadous R., Fatnassi M., Grimoud J., Rey C., Roques C., Combes C. (2022) Injectable bone cement containing carboxymethyl cellulose microparticles as a silver delivery system able to reduce implant-associated infection risk. Acta Biomater., 145, 342-357. doi: 10.1016/J.ACTBIO.2022.04.015Jacquart S., Girod-Fullana S., Brouillet F., Pigasse C., Siadous R., Fatnassi M., Grimoud J., Rey C., Roques C., Combes C. (2022) Injectable bone cement containing carboxymethyl cellulose microparticles as a silver delivery system able to reduce implant-associated infection risk. Acta Biomater., 145, 342-357. doi: 10.1016/J.ACTBIO.2022.04.015Jacquart S., Poquillon D., Dechambre G., Cazalbou S., Rey C., Combes C. (2016) Mechanical properties of self-setting composites: Influence of the carboxymethylcellulose content and hydration state. J. Mater. Sci., 51(9), 4296-4305. doi: 10.1007/s10853-016-9739-4Jacquart S., Poquillon D., Dechambre G., Cazalbou S., Rey C., Combes C. (2016) Mechanical properties of self-setting composites: Influence of the carboxymethylcellulose content and hydration state. J. Mater. Sci., 51(9), 4296-4305. doi: 10.1007/s10853-016-9739-4Kobayashi H., Fujishiro T., Belkoff S.M., Kobayashi N., Turner A.S., Seim H.B., Zitelli J., Hawkins M., Bauer T.W. (2009) Long-term evaluation of a calcium phosphate bone cement with carboxymethyl cellulose in a vertebral defect model. J. Biomed. Mater. Res. Part A, 88A(4), 880-888. doi: 10.1002/jbm.a.31933Kobayashi H., Fujishiro T., Belkoff S.M., Kobayashi N., Turner A.S., Seim H.B., Zitelli J., Hawkins M., Bauer T.W. (2009) Long-term evaluation of a calcium phosphate bone cement with carboxymethyl cellulose in a vertebral defect model. J. Biomed. Mater. Res. Part A, 88A(4), 880-888. doi: 10.1002/jbm.a.31933Krokhicheva P.A., Goldberg M.A., Fomin A.S., Khayrutdinova D.R., Antonova O.S., Baikin A.S., Konovalov A.A., Leonov A.V., Mikheev I.V., Merzlyak E.M., Kirsanova V.A., Sviridova I.K., Sergeeva N.S., Barinov S.M., Komlev V.S. (2023) Enhanced bone repair by silver-doped magnesium calcium phosphate bone cements. Ceramics Int. doi: 10.1016/j.ceramint.2023.03.052Krokhicheva P.A., Goldberg M.A., Fomin A.S., Khayrutdinova D.R., Antonova O.S., Baikin A.S., Konovalov A.A., Leonov A.V., Mikheev I.V., Merzlyak E.M., Kirsanova V.A., Sviridova I.K., Sergeeva N.S., Barinov S.M., Komlev V.S. (2023) Enhanced bone repair by silver-doped magnesium calcium phosphate bone cements. Ceramics Int. doi: 10.1016/j.ceramint.2023.03.052Lee H.J., Kim B., Padalhin A R., Lee B.T. (2019) Incorporation of chitosan-alginate complex into injectable calcium phosphate cement system as a bone graft material. Mater. Sci. Engin. C, 94, 385-392. doi: 10.1016/j.msec.2018.09.039Lee H.J., Kim B., Padalhin A R., Lee B.T. (2019) Incorporation of chitosan-alginate complex into injectable calcium phosphate cement system as a bone graft material. Mater. Sci. Engin. C, 94, 385-392. doi: 10.1016/j.msec.2018.09.039Li C., Hao W., Wu C., Li W., Tao J., Ai F., Xin H., Wang X. (2020) Injectable and bioactive bone cement with moderate setting time and temperature using borosilicate bio-glass-incorporated magnesium phosphate. Biomed. Mater., 15(4), 045015. doi: 10.1088/1748-605X/AB633FLi C., Hao W., Wu C., Li W., Tao J., Ai F., Xin H., Wang X. (2020) Injectable and bioactive bone cement with moderate setting time and temperature using borosilicate bio-glass-incorporated magnesium phosphate. Biomed. Mater., 15(4), 045015. doi: 10.1088/1748-605X/AB633FLiu W.C., Wang H.Y., Chen L.C., Huang S.W., Wu C., Chung R.J. (2019) Hydroxyapatite/tricalcium silicate composites cement derived from novel two-step sol-gel process with good biocompatibility and applications as bone cement and potential coating materials. Ceramics Int., 45(5), 5668-5679. doi: 10.1016/j.ceramint.2018.12.032Liu W.C., Wang H.Y., Chen L.C., Huang S.W., Wu C., Chung R.J. (2019) Hydroxyapatite/tricalcium silicate composites cement derived from novel two-step sol-gel process with good biocompatibility and applications as bone cement and potential coating materials. Ceramics Int., 45(5), 5668-5679. doi: 10.1016/j.ceramint.2018.12.032Miehle E., Bader-Mittermaier S., Schweiggert-Weisz U., Hauner H., Eisner P. (2021) Effect of physicochemical properties of carboxymethyl cellulose on diffusion of glucose. Nutrients, 13(5). doi: 10.3390/nu13051398Miehle E., Bader-Mittermaier S., Schweiggert-Weisz U., Hauner H., Eisner P. (2021) Effect of physicochemical properties of carboxymethyl cellulose on diffusion of glucose. Nutrients, 13(5). doi: 10.3390/nu13051398Rahman M.S., Hasan M.S., Nitai A.S., Nam S., Karmakar A.K., Ahsan M.S., Shiddiky M.J.A., Ahmed M.B. (2021) Recent developments of carboxymethyl cellulose. Polymers, 13(8), 1345. doi: 10.3390/POLYM13081345/S1Rahman M.S., Hasan M.S., Nitai A.S., Nam S., Karmakar A.K., Ahsan M.S., Shiddiky M.J.A., Ahmed M.B. (2021) Recent developments of carboxymethyl cellulose. Polymers, 13(8), 1345. doi: 10.3390/POLYM13081345/S1Shelekhov E.V, Sviridova T.A. (2000) PROGRAMS FOR X-RAY ANALYSIS OF POLYCRYSTALS. Temlicheskaya Obrabotka Metallov, 42(8).Shelekhov E.V, Sviridova T.A. (2000) PROGRAMS FOR X-RAY ANALYSIS OF POLYCRYSTALS. Temlicheskaya Obrabotka Metallov, 42(8).Wang Q., Dong, J. F., Fang, X., & Chen, Y. (2022). Application and modification of bone cement in vertebroplasty : A literature review. Joint Diseases and Related Surgery, 33(2), 467-478. doi: 10.52312/jdrs.2022.628Wang Q., Dong, J. F., Fang, X., & Chen, Y. (2022). Application and modification of bone cement in vertebroplasty : A literature review. Joint Diseases and Related Surgery, 33(2), 467-478. doi: 10.52312/jdrs.2022.628Wang, X.H., Jia S.J., Hao D.J., Wang N.N. (2020) Advances in the modification of injectable calcium-phosphate-based bone cements for clinical application. Chin. Med. J., 133(21), 2610-2612. doi: 10.1097/CM9.0000000000001092Wang, X.H., Jia S.J., Hao D.J., Wang N.N. (2020) Advances in the modification of injectable calcium-phosphate-based bone cements for clinical application. Chin. Med. J., 133(21), 2610-2612. doi: 10.1097/CM9.0000000000001092Wei J., Jia J., Wu F., Wei S., Zhou H., Zhang H., Shin J.W., Liu C. (2010) Hierarchically microporous/macroporous scaffold of magnesium-calcium phosphate for bone tissue regeneration. Biomaterials, 31(6), 1260-1269. doi: 10.1016/j.biomaterials.2009.11.005Wei J., Jia J., Wu F., Wei S., Zhou H., Zhang H., Shin J.W., Liu C. (2010) Hierarchically microporous/macroporous scaffold of magnesium-calcium phosphate for bone tissue regeneration. Biomaterials, 31(6), 1260-1269. doi: 10.1016/j.biomaterials.2009.11.005Wei L., Chen C., Hou Z., Wei H. (2016) Poly (acrylic acid sodium) grafted carboxymethyl cellulose as a high performance polymer binder for silicon anode in lithium ion batteries. Sci. Rep., 6. doi: 10.1038/srep19583Wei L., Chen C., Hou Z., Wei H. (2016) Poly (acrylic acid sodium) grafted carboxymethyl cellulose as a high performance polymer binder for silicon anode in lithium ion batteries. Sci. Rep., 6. doi: 10.1038/srep19583Wu F., Su J., Wei J., Guo H., Liu C. (2008) Injectable bioactive calcium-magnesium phosphate cement for bone regeneration. Biomed. Mater., 3(4). doi: 10.1088/1748-6041/3/4/044105Wu F., Su J., Wei J., Guo H., Liu C. (2008) Injectable bioactive calcium-magnesium phosphate cement for bone regeneration. Biomed. Mater., 3(4). doi: 10.1088/1748-6041/3/4/044105

The authors declare that there are no conflicts of interest present.