食品科学 ›› 2020, Vol. 41 ›› Issue (10): 238-245.doi: 10.7506/spkx1002-6630-20190423-310

• 工艺技术 • 上一篇    下一篇

太平洋牡蛎壳制备L-天冬氨酸螯合钙的工艺优化及表征

王真,姜岁岁,张帆,王润芳,冯雪,汪瑞,李诗洋,赵元晖   

  1. (中国海洋大学食品科学与工程学院,山东 青岛 266003)
  • 出版日期:2020-05-25 发布日期:2020-05-15
  • 基金资助:
    “十三五”国家重点研发计划重点专项(2018YFD0901005);山东省重点研发计划项目(2018GHY115012); 山东省自然科学基金项目(ZR2015CM011)

Optimized Preparation and Characterization of Calcium-chelating L-Aspartate with Pacific Oyster (Crassostrea gigas) Shells as Calcium Source

WANG Zhen, JIANG Suisui, ZHANG Fan, WANG Runfang, FENG Xue, WANG Rui, LI Shiyang, ZHAO Yuanhui   

  1. (College of Food Science and Engineering, Ocean University of China, Qingdao 266003, China)
  • Online:2020-05-25 Published:2020-05-15

摘要: 以太平洋牡蛎壳为钙源,利用电感耦合等离子体质谱测定牡蛎壳中重金属元素含量,采用不同处理方式制备L-天冬氨酸螯合钙,以螯合率和得率为衡量指标进行综合评价,选出最佳处理方式,并进一步分级操作,通过单因素试验从pH值、温度、时间、物质的量比4 个方面对螯合工艺进行综合评分,利用正交试验优化制备条件,且通过能谱分析对产物进行表征研究。结果表明,在煅烧、直接过筛和球磨3 种处理方式下,直接过筛的壳粉与L-天冬氨酸的螯合率显著高于煅烧和球磨处理。对过筛壳粉进一步分级发现,300~200 目筛的壳粉与L-天冬氨酸的螯合率较高。根据单因素试验得到螯合钙的最佳工艺参数为pH 4.5、反应温度50 ℃、反应时间100 min、L-天冬氨酸与Ca2+物质的量比2∶1,此条件下的螯合率高达98.5%。通过扫描电子显微镜、比表面积表征可知,煅烧、直接过筛和球磨3 种处理方式壳粉的微观形态差异较大,且比表面积逐次升高,与各自螯合率的大小相对应。螯合物能谱图结果显示钙元素成功螯合到L-天冬氨酸上。研究结果为废弃牡蛎壳的高值化利用及L-天冬氨酸螯合钙的生产工艺提供理论基础和新的思路。

关键词: 牡蛎壳, 处理方式, L-天冬氨酸螯合钙, 工艺优化

Abstract: The content of heavy metals in Pacific oyster shells was determined by inductively coupled plasma mass spectrometry (ICP-MS), confirming its potential as an excellent calcium source. This material was used to prepare calcium-chelating L-aspartate after being subjected to different pretreatments. The optimal pretreatment was selected based on the chelation efficiency and the product yield, and the resulting powder was fractionated by sieving. The preparation conditions including pH, temperature, time and molar ratio between L-aspartate and Ca2+ were optimized by one-factor-at-a-time and orthogonal array design methods. The obtained chelate was characterized by energy disperse spectrometry (EDS). The results showed that the chelating efficiency of oyster shell powder prepared by sequential grinding and sieving was higher than that of calcined and ball-milled shell powders. The fraction passing through 300–200 had the highest chelating rate with L-aspartate. The optimal conditions for preparing calcium-chelating L-aspartate were determined as follows: pH 4.5, 50 ℃, 100 min, and molar ratio of L-aspartate to Ca2+ 2:1. Under these condition, the chelation rate was as high as 98.5%. According to their scanning electron micrographs (SEM) and BET specific surface area characterization, the morphology of calcined, sieved and ball-milled shell powders was quite different, and their specific surface area increased in that order, corresponding to their respective chelation rates. The EDS results showed that calcium was successfully chelated to L-aspartate. This research provides a theoretical basis and new ideas for the value-added utilization of oyster shell waste and the production of calcium-chelating L-aspartate.

Key words: oyster shell, processing methods, calcium-chelating L-aspartate, process optimization

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