大果木姜子油SFE-CO_(2)萃取工艺及其质量评价方法研究  

Study on SFE-CO_(2)Extraction Process of Cinnamomum Migao Oil and Quality Evaluation Method

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作  者:屠国丽 林岳 钟慧丽 徐文静 严诗楷[4] 马贤鹏 TU Guo-li;Lin Yue;ZHONG Hui-li;XU Wen-jing;YAN Shi-kai;MA Xian-peng(Guizhou Jingcheng Pharmaceutical Co.,Ltd.,Guiyang 550200,China;School of Traditional Chinese Medicine,Guangdong Pharmaceutical University,Guangzhou 510006,China;Shanghai Jingfeng Pharmaceutical Co.,Ltd.,Shanghai 201908,China;School of Pharmacy,Shanghai Jiao Tong University,Shanghai 200240,China)

机构地区:[1]贵州景诚制药有限公司,贵州贵阳550200 [2]广东药科大学中药学院,广东广州510006 [3]上海景峰制药有限公司,上海201908 [4]上海交通大学药学院,上海200240

出  处:《化学试剂》2021年第10期1329-1336,共8页Chemical Reagents

基  金:贵州省科技计划项目(黔科合支撑[2018]2831)。

摘  要:优化大果木姜子油超临界(SFE)-CO_(2)萃取工艺,建立大果木姜子油基于指纹图谱和化学模式识别的质量评价方法。基于单因素试验,以大果木姜子油的萃取率为考察指标,并结合响应面法综合优化SFE-CO2萃取条件。采用Pntulips? QS-C18(4.6 mm×250 mm, 5μm)色谱柱,乙腈-0.4%乙酸为流动相,梯度洗脱,流速0.8 mL/min,柱温25℃,检测波长240 nm,建立大果木姜子油HPLC指纹图谱,利用指纹图谱相似度,以及主成分分析(PCA)、正交偏最小二乘法-判别分析(OPLS-DA)评价10批大果木姜子油产品质量。SFE-CO_(2)最优萃取条件为:萃取压力15 MPa,萃取温度35℃,萃取时间64 min,分离釜Ⅰ压力14 MPa。标定大果木姜子油HPLC指纹图谱中的15个共有特征峰,国家药典委员会指纹图谱评价系统得出各批产品指纹图谱相似度大于0.950,PCA对其质量进一步评价,聚类结果显示10批样本为一类,可见大果木姜子油萃取工艺稳定可控。优化得出大果木姜子SFE-CO_(2)最佳萃取工艺参数,所建立的HPLC指纹图谱可有效表征多批次大果木姜子油的质量特征,为大果木姜子油的生产和质量评价提供研究基础。The supercritical fluid(SFE)-CO_(2)extraction process of Cinnamomum Migao oil was optimized,and its quality evaluation methodology based on fingerprints and chemical pattern recognition was established.Single factor experiments combined with response surface design were used to obtain the optimum extraction conditions for supercritical CO_(2)extraction based on its extraction rate.The fingerprints were analyzed by HPLC on a Pntulips■QS-C18(4.6 mm×250 mm,5μm)column with mobile phase consisted of acetonitrile-0.4%acetic acid solution(gradient elution)at a flow rate of 0.8 mL/min.The detection wavelengths were set at 240 nm and the temperature was set at 25℃.Quality evaluation on 10 batches Cinnamomum Migao oil products were conducted via their fingerprint similarity,and as well on results of principal component analysis(PCA)and orthogonal partial least square discriminate analysis(OPLS-DA)on data of fingerprints.The optimal process conditions for Cinnamomum Migao oil were as follows:extration pressure 15 MPa,extraction temperature 35℃,extraction time 64 mins,and separation pressure 14 MPa.HPLC fingerprint of Cinnamomum Migao oil was established successfully and 15 common characteristic peaks were assigned.Fingerprints have over 0.950 similarities;PCA was further applied to evaluate the quality,and 10 batches of samples were classified into one category,which indicated that the extraction process is stable and controllable.Optimum SFE-CO_(2)extraction process parameters of Cinnamomum Migao oil were proposed,and the established HPLC fingerprinting can effectively describe the quality characteristics of multiple batches of Cinnamomum Migao oil.This study provides scientific basis for the production and quality evaluation of Cinnamomum Migao oil.

关 键 词:大果木姜子油 超临界CO_(2)萃取 指纹图谱 主成分分析 质量评价 

分 类 号:R917[医药卫生—药物分析学]

 

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