Analytical study of osteoporosis of maxilla in ovariectomized rats

ANALYTICAL STUDY OF OSTEOPOROSIS OF MAXILLA IN OVARIECTOMIZED RATS Shifeier Lu BSc Principle Supervisor: Yin Xiao Associate Supervisor: Ross Crawford Submitted in fulfilment of the requirements for the degree of Master of Applied Science (Research) Institute of Health and Biomedical Innovation School of Chemistry, Physics and Mechanical Engineering (CPME) Faculty of Science and Engineering Queensland University of Technology September, 2015 Keywords Bone Osteoporosis Maxilla Scanning electron microscopy (SEM) Energy-dispersive X-ray spectroscopy (EDS) Transmission electron microscope (TEM) Laser ablation inductively coupled plasma mass spectrometer (LA-ICP-MS) Mineralization Ca/P ratio Osteocyte Collagen structure Mineral crystal Trace element Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats i Abstract Bone is mainly composed of supporting cells, organic matrix (made up of collagen and noncollagen proteins), and inorganic mineral (deposited within the matrix) The quality of bone mainly depends on its structural and material properties which include bone mineralization, collagen properties and element distribution As a common chronic skeletal disorder, osteoporosis (OP) leads to the increased risk of bone fractures OP is characterized by reduced bone mass and density and altered micro-architecture To investigate the degree of mineralization of bone and bone mineral density distribution, advanced microscopes and analytical facilities have been applied to observe the morphology and structure of bone at micro and nano scale and measure the composition even at trace level The aims of this study were to apply analytical facilities to investigate the influence of osteoporosis in maxillary bone of ovariectomized rats in both newly formed and mature (old) bone area, and to further optimise the experimental conditions for future relevant analytical studies The maxillary bone samples were collected from normal (Sham) and ovariectomized (Ovx) rat models The composition of mineral was measured by energy-dispersive X-ray spectroscopy (EDS) combined with scanning electron microscopy (SEM) The distribution of trace elements was measured by laser ablation inductively coupled plasma mass spectrometer (LA-ICP-MS) The structure of collagen and mineral crystal was observed and investigated by transmission electron microscope (TEM) and selected area electron diffraction (SAED) patterns The results of EDS showed that the ratio of Ca/P in maxillary bone was comparable between the Ovx and Sham groups, while the observation by TEM and SAED patterns demonstrated that mineral mono crystallites might exist in the Ovx group Using LA-ICP-MS, the concentrations of Zn was detected higher in normal bone than osteoporotic bone The concentrations of Zn, Sr and Pb were higher in mature (old) bone than in newly formed bone while the concentration of Fe was lower in both the Sham and Ovx groups In this study, the difference of metallic and nonmetallic elements in ovariectomy-induced osteoporosis tibia (trabecular bone), maxilla (cortical bone) and normal bone was also investigated by LA-ICP-MS It was ii Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats noted that the concentrations of 28Si, 77 Se, 208 Pb, and Ca/P ratio were higher in tibia and maxilla in osteoporotic rats than those in normal bone at all evaluated timepoints The average concentrations of 88 Sr, 137 Ba, and 208 25 Mg, 28 Si, 39 K, 47 Ti, 56 Fe, 59 Co, 66 Zn, 77 Se, Pb were generally higher in tibia than those in maxilla, indicating tibial trabecular bones may be more sensitive to the change of estrogen than maxillary cortical bones This study demonstrated that the composition of mineral in maxilla was similar between Ovx and Sham groups; however, the changes of maxilla after Ovx treatment occurred in the trace elements and ultrastructure at the nano-scale during bone maturation Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats iii Table of Contents Keywords i Abstract ii Table of Contents iv List of Figures vi List of Tables vii List of Abbreviations viii Statement of Original Authorship x Acknowledgements xi Chapter 1: Introduction 1.1 Background 1.2 Purposes Chapter 2: Literature Review 2.1 Basic Bone Biology 2.1.1 Physiology of Bone 2.1.2 Bone Remodelling and Bone Cells 2.1.3 Jaw Bone 2.2 Process of Biomineralization in Physiological Condition 2.2.1 Biomineralization 2.2.2 Hydroxyapatite 2.2.3 Bone Mineralization 2.3 Osteoporosis and the Alteration of Mineralization in Bone Disease 11 2.3.1 Osteoporosis 11 2.3.2 Alteration of Mineralization in Osteoporosis 14 2.4 The Structure and Role of Collagen in Mineralization 14 2.4.1 The Role of Collagen in Bone 14 2.4.2 The Structure of Type I Collagen 16 2.5 Trace Elements in Bone Metabolism 17 2.6 Methods to Investigate Mineralization in Bone 19 Chapter 3: Research Design 23 3.1 Methodology 23 3.2 Measurement of Bone Mineral Composition 24 3.2.1 Scanning Electron Microscope 24 3.2.2 Energy Dispersive X-ray Spectroscopy 25 3.2.3 Sample Preparation 25 3.2.4 Sample Measurement 26 3.3 Observation of Bone Collagen and Mineral Crystal 26 3.3.1 Transmission Electron Microscope 26 3.3.2 Sample Preparation 27 3.3.3 Observation of Collagen and Mineral with TEM 27 iv Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats 3.3.4 Selected Area Electron Diffraction 27 3.3.5 Observation of Mineral Distribution of Mineral Crystal 28 3.4 Measurement of Trace Elements Distribution 28 3.4.1 Laser Ablation Inductively Coupled Plasma Mass Spectrometer 28 3.5 Trace Elements Measurement with LA-ICP-MS 29 3.6 Statistical Analysis 30 Chapter 4: Results 31 4.1 Results of SEM observation and measurement 31 4.1.1 Backscattered Electron Imaging of Bone 31 4.1.2 Mineralization Density Analyses 34 4.2 Results of TEM observation 36 4.2.1 Effect of Ovx on bone collagen and apatite crystals 36 4.3 Results of LA-ICP-MS Measurement 38 4.3.1 Elements distribution assessed by LA-ICP-MS 38 4.3.2 Ca/P ratio of tibia and maxilla 38 4.3.3 The effect of Ovx on the average concentrations of atomic minerals in tibia and maxilla at defined time points 39 4.3.4 The concentrations of atomic minerals, 59Co and 208Pb, in tibia and maxilla 41 4.3.5 The effect of Ovx on the concentrations of 66Zn, 88Sr and 137Ba in tibia and maxilla 43 4.3.6 The difference of trace elements between new bone and old bone 46 Chapter 5: Discussion 48 5.1 The mineral composition of osteoporotic maxilla 48 5.2 The distribution of trace elements in osteoporotic maxilla 49 5.3 The structure of collagen and mineral crystal in osteoporotic maxillary bone 53 5.4 The application of analytical facilities and experimental conditionS 54 Chapter 6: Conclusions 55 Bibliography 56 Appendices 69 List of Publications and Presentations 69 Ethic Approval for Samples Involved in This Project 71 Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats v List of Figures Figure Crystal lattice structure Figure The hydroxyapatite unit cell Figure Sketches of the hierarchical levels of typical cortical bone 10 Figure The structure of collagen fibre at different levels 16 Figure Method used to distinguish the newly formed bone and old bone 32 Figure Area of interest of newly formed bone and old bone 33 Figure (a-d) Element compositions as representative spectra from energy dispersive X-ray (EDS) analysis (e) Summary of Ca/P ratio of the samples measured by EDS 35 Figure TEM micrographs of longitudinally-sectioned mineralized collagen fibrils and selected area electron diffraction (SAED) patterns 37 Figure The Ca/P ratio values (normalised against matrix-matched reference materials) in tibia and maxilla increased after ovariectomy at different time points post-surgery 38 Figure 10 Summary of Ca/P ratio of the new bone and old bone in maxilla measured by LA-ICP-MS 39 Figure 11 The average concentrations of 208Pb (normalised against matrixmatched reference materials) for both tibia and maxilla at all timepoints post-surgery 41 Figure 12 The average concentrations of 59Co in tibia and maxilla at different time points after the surgery 42 Figure 13 The average concentrations of 66Zn in both tibia and maxilla after normalised against matrix-matched reference materials at different time points post-surgery 43 Figure 14 The average concentrations of 88Sr in tibia at different time points after the surgery 44 Figure 15 The average concentration of 137Ba in both tibia and maxilla at different time points post-surgery 45 Figure 16 Element distribution of each group measured by LA-ICP-MS 47 vi Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats List of Tables Table The functions of trace elements in bone metabolism 19 Table ICP-MS operating conditions 30 Table The effect of Ovx on the average concentrations of atomic minerals in tibia and maxilla over time 40 Table Element distribution of each group measured by LA-ICP-MS 46 Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats vii List of Abbreviations Ba Barium BMD Bone mineral density BMDD Bone mineral density distribution C Carbon Ca Calcium Co Cobalt CP Cross polarization DEXA Dual-energy X-ray absorptiometry ECM Extracellular matrix EDS Energy dispersive spectrometry Fe Iron FTIRI Fourier transform infrared imaging H Hydrogen HR High-resolution HSD Honest significant differences K Potassium LA-ICP-MS Laser ablation inductively coupled plasma mass spectrometry MAS Magic angle spinning Mg Magnesium MRI Magnetic resonance imaging NMR Nuclear magnetic resonance SAED Selected area electron diffraction SAXS Small-angle X-ray Scattering SD Standard deviations Se Selenium SEM Scanning electron microscope Si Silicon Sr Strontium TEM Transmission electron microscope Ti Titanium OP Osteoporosis viii Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 58 Bonewald, L.F., The amazing osteocyte 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(Manuscript in preparation) Jun Wang, Ali Kalhor, Shifeier Lu, Ross Crawford, Jiang-Dong Ni, Yin Xiao “iNOS expression and osteocyte apoptosis in idiopathic, nontraumatic osteonecrosis.” Acta orthopaedica 85, no (2014): 1-8 Qiliang Zuo, Thor Friis, Shifeier Lu, Zhibin Du, Ross Crawford, Jiangwu Yao, Yin Xiao “Characterization of nano-structural and nano-mechanical properties of osteoarthritic subchondral bone.” (Under review) The following is a list of conference presentations during the Master candidature: Shifeier Lu, Pingping Han, Zhibin Du, Qiliang Zuo, Ross Crawford, Yin Xiao “Ultrastructural Analysis of Maxilla Bone Mineralization in Rat Osteoporosis Model.” Asia-Pacific Tissue Engineering and Regenerative Medicine International Society (TERMIS-AP) 24th-27th September 2014, Daegu, Republic of Korea Oral Presentation Shifeier Lu, Pingping Han, Zhibin Du, Qiliang Zuo, Ross Crawford, Yin Xiao “Analysis in Ultrastructure of Maxilla Bone Mineralization in Rat Ovx Model.” IHBI Inspires 20th-21st November Gold Coast, Australia Poster Presentation Appendices 69 Qiliang Zuo, Jiangwu Yao, Shifeier Lu, Zhibin Du, Wei Shi, Yin Xiao “Protein-bound phosphate function in collagen mineralization.” AsiaPacific Tissue Engineering and Regenerative Medicine International Society (TERMIS-AP) 24th-27th September 2014, Daegu, Republic of Korea Poster Presentation 70 Appendices Appendix B Ethic Approval for Samples Involved in This Project Appendices 71 72 Appendices ... (LA-ICP-MS) Mineralization Ca/P ratio Osteocyte Collagen structure Mineral crystal Trace element Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats i Abstract Bone is mainly composed of. .. TEM 27 iv Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats 3.3.4 Selected Area Electron Diffraction 27 3.3.5 Observation of Mineral Distribution of Mineral Crystal... List of Publications and Presentations 69 Ethic Approval for Samples Involved in This Project 71 Analytical Study of Osteoporosis of Maxilla in Ovariectomized Rats v List of Figures