[关键词]
[摘要]
目的 针对目前岩藻多糖制备工艺中存在周期长、成本高昂、污染环境的问题,开发一种更为绿色高效的岩藻多糖制备新工艺。方法 新工艺不使用有机溶剂,采用“多段变温提取、酸化、脱色、透析、真空干燥”步骤制备岩藻多糖。以岩藻多糖质量分数和产率作为工艺评价指标,通过鱼骨图以及失效模式与影响分析辨析潜在的关键工艺参数(critical process parameters,CPPs)。使用确定性筛选实验设计(definitive screening design,DSD)确定CPPs为提取温度、提取时间、液固比、透析相对分子质量、脱色时间。建立CPPs和工艺评价指标之间的定量数学模型。基于蒙特卡罗方法计算不同工艺参数条件下的风险值,根据风险阈值确定设计空间并进行实验验证。结果 优化所得岩藻多糖制备工艺参数范围为液固比14~22 mg/mL,提取温度75~85 ℃,提取时间为26~30 min,脱色时间为30~40 min,透析相对分子质量为1 000~6 000;所得岩藻多糖质量分数>75%,产率>3%。新工艺绿色度得分达到77分,高于传统酸提取工艺的59分。结论 新工艺能够得到高纯度岩藻多糖,符合绿色发展理念,有良好工业转化前景。
[Key word]
[Abstract]
Objective To develop a greener and more efficient fucoidan preparation process addressing the current challenges of long production cycles, high costs, and environmental pollution in existing methods. Methods The novel process eliminates organic solvents and employs sequential steps to prepare fucoidan: multi-stage temperature-varied extraction, acidification, decolorization, dialysis, and vacuum drying. Fucoidan mass fraction and yield were selected as process evaluation criteria. Fishbone diagrams and failure mode and effects analysis were utilized to identify potential critical process parameters (CPPs). A definitive screening design (DSD) was used to confirm the CPPs as extraction temperature, extraction time, liquid-to-solid ratio, dialysis molecular weight cutoff, and decolorization time. Quantitative mathematical models were established to CPPs with evaluation criteria. Risk values under varying parameter conditions were calculated using Monte Carlo simulations, and the design space was determined based on risk thresholds, followed by experimental validation. Results Optimized process parameters included a liquid-to-solid ratio of 14—22 mg/mL, extraction temperature of 75—85 ℃, extraction time of 26—30 min, decolorization time of 30—40 min, and dialysis molecular weight cutoff of 1 000—6 000. The resulting fucoidan exhibited mass fraction > 75% and yield > 3%. The greenness score of the novel process reached 77, surpassing the 59 score of conventional acid extraction. Conclusion The developed process achieves high-purity fucoidan, aligns with green manufacturing principles, and demonstrates strong potential for industrial-scale application.
[中图分类号]
R283.6
[基金项目]
国家重点研发计划项目(2024YFC3506901);浙江省“尖兵领雁+X”科技计划项目(2025C02088);技术开发委托合同(XH-2022-KYC-210000-0001);金华市公益性技术应用研究项目(2023-4-188)