超声辅助脱脂对牦牛骨粉制备及其理化特性的影响

    Effect of ultrasonic-assisted degreasing on preparation and physicochemical properties of yak bone powder

    • 摘要: 为提高牦牛骨粉的脱脂率,以青海牦牛股骨为原料进行超声辅助有机溶剂脱脂参数优化,并比较分析了超声脱脂法和蒸煮脱脂法对骨粉制备的影响。该文以脱脂率为指标筛选高效脱脂溶剂;通过响应面法对超声脱脂参数(超声功率、脱脂时间及液料比)进行优化;对比分析了2种脱脂牦牛骨的脱脂率、蛋白质流失率、主要矿物质流失率、微观形态及其骨粉的粒径分布、微观形态、化学结构和钙离子释放度。结果显示:乙酸乙酯为最佳脱脂溶剂;超声功率500 W,超声时间30 min,液料比(体积质量比)6为最佳脱脂参数,此条件下脱脂率达92.00%,显著高于蒸煮脱脂法(71.25%)(P<0.01);与蒸煮脱脂法相比,超声脱脂法蛋白质流失率(8.11%),主要矿物质元素Na、K、Fe、Mn流失率显著降低(P<0.05),微观结构更加致密;超声脱脂法和蒸煮脱脂法制得牦牛骨粉中值粒径(D50)分别为35.84 μm和11.73 μm;红外光谱显示两者化学结构无明显变化;钙离子释放度结果显示两者同样无显著差异(P>0.05)。超声波辅助有机溶剂脱脂处理制备骨粉可更多保留骨中营养物质,对改善骨粉加工工艺及提高骨粉品质具有一定的参考价值。

       

      Abstract: Abstract: In order to reduce the degreasing rate and improve the quality of yak bone powder, the ultrasonic assisted organic solvent degreasing method was studied based on the thighbone of Qinghai yak in this paper, and the nutrient contents and physicochemical properties were analyzed comparing with the traditional boiling degreasing method. Firstly, the degreasing solvent was screened according to degreasing rate and applicability among four common organic solvents. Basing on the single factor test, Box-Behnken test was designed to optimize the parameters including ultrasonic power, degreasing time and the ratio of liquid to material. After that, the analysis of the degreasing rate, the loss rate of protein, collagen, main minerals and the microstructure of yak bone treated by ultrasonic and boiling was carried out. Subsequently, the particle size distribution, microstructure, chemical structure and calcium release rate of yak bone powder dealt with the planetary ball mill were shown as well. Results suggested that ethyl acetate was the optimal degreasing solvent with a higher degreasing rate and better applicability under the same conditions. In addition, the two regression model built by response surface design had a good fitting degree with the correlation coefficient of 0.9484 indicating that the model fitted well in the whole regression region. Considering the energy consumption, the optimum degreasing conditions were finally determined as follows: ultrasonic power is 500 W, ultrasonic time is 30min, and the ratio of liquid to material (mL/g) is 6, under which conditions the degreasing rate could reach 92.00%±0.20% and the relative error of the predicted value was 1.08% which was less than 5% revealing that the model was effective. Besides that, it was also found that the degreasing rate of ultrasonic (92.00%±0.20%) was significantly higher than that of boiling method (71.25%±2.31%) (P<0.05). Meanwhile, the loss rate of protein and collagen were 8.11%±0.48%, 11.05%±2.45%, respectively, which were dramatically lower (P<0.05). And there was a serious loss of Na, K, Fe, Mn in cooked yak bone that were 19.00%±1.44%, 58.95%±1.04%, 14.32%±2.46% and 20.86%±1.29% respectively while the loss about Fe, Zn, Mn in ultrasonic skimmed yak bone was slightly, and the contents of P, Ca, Mg, Cu, Se, Mo, Sr in the bone treated with the two methods were similar (P>0.05). As for the microstructure of yak bone, the boiling one was looser and more porous. After pulverization, the median diameter of ultrasonic defatted bone powder was (35.84±0.60) μm while the other was (11.73± 0.29) μm, which was in agreement with the result of scanning electron microscope. Moreover, no significant difference had been observed in the chemical structure, and there were mainly phosphate and carbonate in two kinds of bone powder. For the calcium release rate of bone powder, result indicated that both methods had no significant difference (P>0.05). In conclusion, the ultrasonic assisted organic solvent degreasing method could remain more nutrients with the higher degreasing rate. This study provided a high efficient degreasing method, which has the value for improving the processing technology for preparing the yak bone powder.

       

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