化橘红药材挥发油提取及用饱和水溶液法包合工艺研究

王文平，尹兴斌，董晓旭，杨春静，张海英，游龙泰，倪健

北京中医药大学中药学院，北京 100102

摘要：目的 优选化橘红药材挥发油提取及包合的最佳工艺。方法 以挥发油得率为指标，采用单因素试验考察挥发油的提取工艺；以挥发油包合率及包合物得率为评价指标，采用饱和水溶液法，进行 L9（34）正交试验，优选挥发油的包合工艺，并采用显微呈像分析、X射线衍射法对包合物进行表征。结果 挥发油的最佳提取工艺为不浸泡，加10倍量水，提取10 h；最佳包合工艺为：油（mL）∶β-环糊精（g）∶水（mL）＝

1∶8∶80，包合温度为 50 ℃，包合时间为3 h。包合工艺的验证试验显示，挥发油包合率、包合物得率平均值分别为 91.50%、88.36%。显微镜法、X 射线衍射法表明包合物形成，包合物状态良好。结论 本试验优选出的挥发油提取及包合工艺稳定可行，可为制剂生产提供一定依据。关键词：化橘红；挥发油；提取；β-环糊精；包合工艺

DOI：10.3969/j.issn.1005-5304.2017.11.016

中图分类号：R284.2 文献标识码：A 文章编号：1005-5304(2017)11-0067-04

Study on Extraction and Inclusion Process of Volatile Oil from Citri Grandis Exocarpium with Saturated Aqueous Solution

WANG Wen-ping, YIN Xing-bin, DONG Xiao-xu, YANG Chun-jing, ZHANG Hai-ying, YOU Long-tai, NI Jian (College of Pharmacy, Beijing University of Chinese Medicine, Beijing 100102, China)

Abstract: Objective To optimize the processes of extraction and inclusion of volatile oil from Citri Grandis Exocarpium. Methods With yield ratio of volatile oil as evaluation index, single factor experiments were used to study the extraction process of volatile oil. With the inclusion rate of the volatile oil and the yield of inclusion as evaluation indexes, saturated aqueous solution was used to the L9(34) orthogonal experiments to reach the best inclusion process optimization. And the microscopic imaging analysis and X-ray scattering technology were adopted to character the inclusion compound. Results The optimum extraction process of volatile oil was extracted for 10 hours with 10 folds the amount of water, and without soaking. The optimum conditions of inclusion process were as follows: volatile oil (mL): β-CD (g): water (mL) ratio was 1:8:80; inclusion temperature was 50 ℃; inclusion time was 3 hour. The validation experiments of the inclusion rate of the volatile oil and the yield of inclusion were 91.50% and 88.36%. Microscopic imaging analysis and X-ray scattering technology proved the inclusion compound had been formed. Conclusion Optimal extraction and inclusion process are feasible and stable, which can provide certain supporting data for preparation and production.

Key words: Citri Grandis Exocarpium; volatile oil; extraction; β-CD; inclusion process

化橘红为芸香科植物化州柚 Citrus grandis ‘Tomentosa’或柚 Citrus grandis（L.）Osbeck 的未成熟或近成熟的干燥外层果皮，前者习称“毛橘红”，后者习称“光七爪”“光五爪”，具有理气宽中、燥湿化痰功效，用于治疗咳嗽痰多、食积伤酒、呕恶痞

闷[1-2]。化橘红是广东省道地药材，其主要成分有挥发油、黄酮、多糖等。化橘红的挥发油具有明显的镇咳、祛痰作用，是化橘红的主要活性成分，且出油率

高，在治疗痰症、咳喘的中药复方中出现频率很高[3]。迄今化橘红挥发油的工艺研究鲜有报道，且少数研究

报道为化橘红粗粉的提取工艺[4]，但实际生产中药材粉末提取挥发油易造成挥发油的成分损失且在煎煮过程中易导致糊锅，因此，在实际生产中化橘红为原药材不粉碎入药。目前对于化橘红原药材挥发油的包合工艺尚未见报道。本试验以化橘红原药材为研究对