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中国精品科技期刊2020
陈红斌,洪伦波,汪娟,等. 响应面优化高速剪切法制备薄荷挥发油包合物工艺[J]. 华体会体育,2023,44(22):210−218. doi: 10.13386/j.issn1002-0306.2023020138.
引用本文: 陈红斌,洪伦波,汪娟,等. 响应面优化高速剪切法制备薄荷挥发油包合物工艺[J]. 华体会体育,2023,44(22):210−218. doi: 10.13386/j.issn1002-0306.2023020138.
CHEN Hongbin, HONG Lunbo, WANG Juan, et al. Preparation of Peppermint Oil/β-CD Inclusion by High-speed Shearing with Process Optimization Using ResponseSurface Methodology[J]. Science and Technology of Food Industry, 2023, 44(22): 210−218. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023020138.
Citation: CHEN Hongbin, HONG Lunbo, WANG Juan, et al. Preparation of Peppermint Oil/β-CD Inclusion by High-speed Shearing with Process Optimization Using ResponseSurface Methodology[J]. Science and Technology of Food Industry, 2023, 44(22): 210−218. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023020138.

响应面优化高速剪切法制备薄荷挥发油包合物工艺

Preparation of Peppermint Oil/β-CD Inclusion by High-speed Shearing with Process Optimization Using ResponseSurface Methodology

  • 摘要: 目的:考察高速剪切结合冷冻干燥法制备薄荷挥发油的β-环糊精(β-cyclodextrin,β-CD)包合物的最佳工艺。方法:对比冷冻干燥与真空干燥,高速剪切与搅拌法对包合工艺的影响;在单因素实验基础上,以β-CD与挥发油的比例、包合温度和β-CD的质量分数为影响因素,以含油率和包合率的综合评分为评价指标,考察Box-Behnken响应面法优化的包合工艺;采用高效液相色谱(high performance liquid chromatography,HPLC)测包合物中的胡薄荷酮含量;傅里叶变换红外光谱(fouriertransforminfrared spectroscopy,FTIR)对包合物进行表征。结果:冷冻干燥法制备的包合物收率更高,平均收率为97.6%。高速剪切法制备的含油率和包合率较高,与搅拌法相比分别高出约3%和19%;包合物的最佳制备条件为:β-CD与挥发油比例为9:1(g/mL),包合温度为55 ℃,β-CD的质量分数为17%。在此条件下,挥发油含油率为10.9%,挥发油包合率为97.6%,综合评分为99.7,RSD值为1.59%,优化的工艺稳定可行;通过HPLC测得包合物中胡薄荷酮含量为2.465 mg/g;FTIR分析证明了薄荷油-β-CD包合物的形成。结论:高速剪切和冷冻干燥法结合制备薄荷挥发油包合物效率高,工序简便,提高了收率,对生产工艺有指导作用。

     

    Abstract: Objective: To investigate the optimal process for preparing peppermint essential oil/β-cyclodextrin (β-CD) inclusion complex using high-speed shearing combined with freeze-drying. Methods: The effects of freeze-drying and vacuum drying, high-speed shearing, and stirring on the encapsulation process were compared. Based on single-factor experiments, the ratio of β-CD to essential oil, encapsulation temperature, and mass fraction of β-CD were considered as influencing factors. The comprehensive score of oil content and encapsulation efficiency was used as an evaluation index to investigate the Box-Behnken response surface method for optimizing the encapsulation process. The content of pulegone in the inclusion complex was measured by high-performance liquid chromatography (HPLC). Fourier transform infrared spectroscopy (FTIR) was used to characterize the inclusion complex. Results: The yield of inclusion complex prepared by freeze-drying was higher, with an average yield of 97.6%. The oil content and encapsulation efficiency by the high-speed shearing method were relatively high, being about 3% and 19% higher than those by the stirring method, respectively. The optimized conditions were as follows: The weight ratio of β-CD to volatile oil was 9:1 (g/mL), the encapsulation temperature was 55 ℃, and the mass fraction of β-CD was 17%. Under these conditions, the essential oil content was 10.9%, the encapsulation efficiency was 97.6%, the comprehensive score was 99.7, the RSD value was 1.59%, and the optimized process was stable and feasible. The content of pulegone in the inclusion complex was found to be 2.465 mg/g by HPLC. The formation of the peppermint oil/β-CD inclusion complex was confirmed by analysis using FTIR. Conclusion: The combination of high-speed shearing and freeze-drying for the preparation of peppermint essential oil inclusion complex had the advantages of high efficiency, simple process, and it improved theyield, would provide guidance for the production process.

     

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