柠檬酸浓度对硼酸盐玻璃骨水泥性能的影响

doi:10.15541/jim20160598

摘要/Abstract

摘要：

以壳聚糖-甘油磷酸钠-柠檬酸溶液为液相, 制备了一种新型可注射的硼酸盐玻璃骨水泥, 通过维卡仪、万能试验机、XRD、FTIR、SEM-EDS等探究了液相中柠檬酸浓度(0.1, 0.2和0.4 g/mL)对硼酸盐玻璃骨水泥性能的影响。结果表明: 柠檬酸浓度显著影响骨水泥的凝结时间和可注射性。柠檬酸浓度为0.2 g/mL时获得的骨水泥的凝结时间最短, 为(16±0.5) min; 可注射性最好, 接近100%。骨水泥压缩强度随柠檬酸浓度增大而增强, 最大可达(26.7±1.9) MPa。SEM照片显示骨水泥中生成了许多纳米微粒。XRD、FTIR和EDS等结果证明, 这些纳米微粒主要是硼酸盐、磷酸盐和柠檬酸盐等物质, 而且柠檬酸浓度能够影响骨水泥中硼酸盐晶体的形成。此外, 柠檬酸能够加速玻璃颗粒在磷酸钠盐缓冲液中的降解速率。

关键词: 柠檬酸, 硼酸盐玻璃, 骨水泥, 性能

Abstract:

A novel injectable borate glass bone cement (BGBC) was prepared by using citric acid-β glycerophosphate-chitosan solution as setting solution. The effect of citric acid (H₃Cit) concentration (0.1, 0.2 and 0.4 g/mL) on the properties of BGBC was investigated by using vicat apparatus, universal testing machine, XRD, FTIR, and SEM-EDS measurements. The experimental results indicate that H₃Cit concentration significantly influences setting time and injectability of BGBC. At the H₃Cit concentration of 0.2 g/mL, BGBC obtains the shortest setting time of (16±0.5) min and best injectability, which is almost fully injectable. It compressive strength increases with the increase of H₃Cit concentration, with the maximum compressive strength up to (26.7±1.9) MPa. SEM images show that a large amount of nanoparticles are formed in the BGBC. XRD, FTIR and EDS results confirm that these nanoparticles contain borates, phosphates and phosphates. Furthermore, formation of borate crystals in the BGBC is influenced by H₃Cit concentration. Immersion experiment of borate glass particles into phosphate buffer with different H₃Cit concentrations shows that the degradation of borate glass is accelerated by H₃Cit.

Key words: citric acid, borate glass, bone cement, property

中图分类号:

TB332

李海滨, 王德平, 吴莹莹, 姚爱华, 叶松. 柠檬酸浓度对硼酸盐玻璃骨水泥性能的影响[J]. 无机材料学报, 2017, 32(8): 831-836.

LI Hai-Bin, WANG De-Ping, WU Ying-Ying, YAO Ai-Hua, YE Song. Effect of Citric Acid Concentration on the Properties of Borate Glass Bone Cement[J]. Journal of Inorganic Materials, 2017, 32(8): 831-836.

图/表 10

表1 样品的液相组成

Table 1 Liquid composition of samples

Sample	H₃Cit/(g·mL^-1)	CS/(g·mL^-1)	GP /(g·mL^-1)
S1	0.1	0.005	0.056
S2	0.2	0.005	0.056
S3	0.4	0.005	0.056

图1 样品的注射曲线

Fig. 1 Injection curve of samples

表2 样品的凝结时间和可注射性

Table 2 Setting time and injectability of samples

Sample	Setting time/min	Injectability/%	Injection force/N
S1	40±2.0	75±7	86.5
S2	16±0.5	>95	28.1
S3	20±1.0	35±10	17.6

图2 样品的压缩强度

Fig. 2 Compressive strength of samples

图3 样品的XRD图谱

Fig. 3 XRD patterns of samples

图4 样品的红外图谱

Fig. 4 Infrared spectra of samples

图5 样品断面的SEM照片((a) S1; (b) S2; (c) S3)和图(b)中红色方框区域的能谱图

Fig. 5 SEM images of the fracture surfaces of samples ((a) S1; (b) S2; (c) S3) and EDS pattern of the boxed area in Fig. (b)

图6 硼酸盐玻璃在PBS-0、PBS-0.1、PBS-0.2和PBS-0.4溶液中的降解曲线(a)以及浸泡液中B离子释放浓度(b)

Fig. 6 Degradation curves of borate glass in the PBS-0, PBS-0.1, PBS-0.2 and PBS-0.4 (a) and the B ion release concentration in the immersion solution (b)

图7 浸泡液的pH随浸泡时间的变化情况

Fig. 7 Variation of pH of immersion solutions with the immersion time

图8 骨水泥凝结机理示意图

Fig. 8 Schematic diagram of setting mechanism of bone cement

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