Nano-hydroxyapatite (n-HAP) from Pangasius bone side streams and its application as a reinforcing agent in biodegradable food packaging films

Oshin Kawduji Thool, Abhilash Sasidharan, Bindu M. Krishna, Sarasan Sabu, Muhammed Navaf and Kappat Valiyapeediyekkal Sunooj
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Abstract

The bone side streams from catfish (Pangasianodon hypophthalmus) were used to produce nano-hydroxyapatite (n-HAP) by a calcination method. Bones were de-proteinized and calcined at 500, 700, and 900 °C at 2, 4, and 9 h, pulverized and cooled. Inductively coupled plasma (ICP-OES), Fourier Transform Infrared (FTIR) spectroscopy, X-ray diffraction (XRD), and Transmission Electron Microscopy (TEM) were used to characterize the trace elements, functional groups, phase formation, and morphology of n-HAP, respectively. Using ICP-OES, an atomic ratio of 1.56 Ca/P was found in catfish bone calcined at 900 °C for 9 h. The FTIR spectra of the sample calcined to the same degree were matched with the standard hydroxyapatite FTIR spectrum. A high crystallinity of 99.5% was confirmed by XRD measurements as the calcination temperature and duration were increased. TEM analysis revealed that the n-HAP crystals have an average size of 71.38 nm. Cassava starch–n-HAP reinforced composite films were prepared with varying n-HAP concentrations which resulted in minor variations in the film thickness ranging from 0.05 to 0.16 mm. The control film exhibited a tensile strength (TS) value of 12.5 MPa while the maximum TS value of 16.10 MPa was exhibited by the sample with 0.8% n-HAP. The lowest elongation at break value was reported for the control film (1.55%) and the maximum (6.87%) was reported for the sample with 0.4% n-HAP. The film incorporating 0.8% n-HAP showed the highest seal strength while the water vapor transmission rate (WVTR) of the composite films reduced from 3.59 × 10−1 g Pa−1 m−1 s−1 to 1.67 × 10−1 g Pa−1 m−1 s−1 as n-HAP concentration increased. The film incorporating 0.4% n-HAP showed identical WVTR values to those of the film with 0.8% n-HAP. These results showed that the n-HAP-incorporating films exhibited better mechanical and barrier properties compared to the control film.

Abstract Image

巴沙鱼骨侧流纳米羟基磷灰石及其在生物可降解食品包装膜中的应用
利用鲶鱼(Pangasianodon hypophthalmus)骨侧流煅烧制备纳米羟基磷灰石(n-HAP)。骨被去蛋白化并在500、700和900°C下煅烧2、4和9小时,粉碎并冷却。利用电感耦合等离子体(ICP-OES)、傅里叶变换红外(FTIR)光谱、x射线衍射(XRD)和透射电子显微镜(TEM)分别表征了n-HAP的微量元素、官能团、相形成和形貌。用ICP-OES测定了900℃煅烧9 h的鲶鱼骨的原子比为1.56 Ca/P,煅烧程度相同的样品的FTIR光谱与标准羟基磷灰石的FTIR光谱相匹配。随着煅烧温度的升高和煅烧时间的延长,煅烧产物的结晶度达到99.5%。TEM分析表明,n-HAP晶体的平均尺寸为71.38 nm。制备了不同n-HAP浓度的木薯淀粉- n-HAP增强复合膜,膜厚度变化较小,在0.05 ~ 0.16 mm之间。对照膜的抗拉强度(TS)为12.5 MPa,而添加0.8% n-HAP的样品的TS最大值为16.10 MPa。对照膜的断裂伸长率最低(1.55%),添加0.4% n-HAP的试样的断裂伸长率最高(6.87%)。随着n-HAP浓度的增加,复合膜的水蒸气透过率(WVTR)从3.59 × 10−1 g Pa−1 m−1 s−1降至1.67 × 10−1 g Pa−1 m−1 s−1,而n-HAP含量为0.8%的复合膜的密封强度最高。含0.4% n-HAP的膜与含0.8% n-HAP的膜的WVTR值相同。这些结果表明,与对照膜相比,加入n- hap的膜具有更好的机械性能和阻隔性能。
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