响应面法优化超临界CO₂萃取决明子挥发油工艺及其抑菌活性研究

目的:采用响应面法对超临界CO₂萃取决明子挥发油的工艺进行优化,同时对提取所得决明子挥发油的抑制活性进行研究,对挥发油成分进行初步分析。方法:在单因素实验基础上,采用中心组合(Box-Behnken)实验设计,考察萃取压力、温度、时间对挥发油提取率的影响,采用响应面分析法对实验结果进行分析,同时采用纸片扩散法对提取所得挥发油抑菌效果进行考察,采用GC-MS法对挥发油成分进行分析。结果:超临界CO₂萃取决明子挥发油的最优提取工艺:萃取温度51℃,萃取压力25 MPa,萃取时间3.22 h;在最优条件下,萃取率可达2.34%;抑菌活性研究结果表明,决明子挥发油对几种常见的细菌和真菌具有较好的抑菌活性,最低抑菌浓度(MIC)在2.5~5 mg·mL^-1范围内。结论:超临界CO₂萃取决明子挥发油工艺稳定,提取率较高,决明子挥发油具有明显的抑菌活性,为其在抑菌制剂中的应用提供了一定的理论依据。

Objective: To adopt the response surface analysis method to optimize the supercritical carbon dioxide extraction conditions of Semen Cassiae volatile oil;to study the antimicrobial activity of the extract from Semen Cassiae, as well as the components of the volatile oil.Methods: The Box-Benhken central composite design method was used based on the single factor experiments.The effects of the temperature, extraction time and on the yield were studied.The response surface method was employed to analyze the results of experiments.The disk diffusion method was used to detect the antimicrobial activity of Semen Cassiae volatile oil.GC-MS was used to analyze the volatile oil components.Results: The results indicated that the optimum extraction conditions were as follows:extraction temperature was at 51℃, extraction pressure was 25 MPa, extraction time was 3.22 h.The extraction yield reached 2.34%.The volatile oil of Semen Cassiae had antimicrobial activity of the tested strains, the MIC of the volatile oil ranged from 2.5 mg·mL^-1 to 5 mg·mL^-1.Conclusion: The supercritical carbon dioxide extraction is a stable and efficient process and the volatile oil of Semen Cassiae had antimicrobial activity.This study could provide certain theoretical basis for application of volatile oil.

[1] 中国药典2010年版. 一部[S].2010:135 ChP 2010.Vol Ⅰ[S].2010:135
[2] 冯年平,沈岚,韩朝阳,等.决明子微波萃取法与常用提取方法的比较[J]. 中成药,2004,26(3):189 FENG NP,SHEN L,HAN CY,et al.Comparative study on the extraction of anthraquinone from Semen Cassiae by MAE and commonly used extraction methods[J].China Tradit Pat Med, 2004,26(3):189
[3] 郝延军,桑育黎,赵余庆,等. 决明子的研究进展[J].中草药, 2001,32(9):858 HAO YJ,SANG YL,ZHAO YQ,et al.The research progress of Semen Cassiae[J].Chin Tradit Herb Drugs,2001,32(9):858
[4] 潘正军,陆祈,潘丽,等.决明子水提液对高血压小鼠血压血脂及肾脏结构的影响[J].中国实验方剂学杂志,2010,16(15):196 PAN ZJ,LU Q,PAN L,et al.Effects of water extracts from Cassia obtusifolia on blood pressure,blood lipid and renal structure in coldinduced hypertensive mice[J].Chin J Exp Tradit Med Form,2010, 16(15):196
[5] SHARMA PR,MONDHE DM,MUTHIAH S,et al.Anticancer activity of an essential oil from Cymbopogon flexuosus[J].Chem Biol Interact,2009,179(2-3):160
[6] LOIZZO MR,TUNDIS R,MENICHINI F,et al.Cytotoxic activity of essential oils from labiatae and lauraceae families against in vitro human tumor models[J].Anticancer Res,2007,27(5A):3293
[7] 李续娥,郭宝江,曾志.决明子蛋白质、低聚糖及蒽醌苷降压作用的实验研究[J].中草药,2003,34(9):842 LI XE,GUO BJ,ZENG Z.Research of the Cassia seed protein, oligosaccharide and anthraquinone glycosides antihypertensive effect from Cassia obtusifolia[J].Chin Tradit Herb Drugs,2003,34(9):842
[8] 徐响,刘光敏,高彦祥. 超临界CO₂ 萃取植物籽油的研究进展[J]. 粮油食品科技,2008,16(1):31 XU X,LIU GM,GAO YX.Research progress on supercritical CO₂ extraction of plant seed oils[J].Sci Technol Cereals Oil Food, 2008,16(1):31
[9] 余小翠,刘高峰. 响应面分析法在中药提取和制备工艺中的应用[J]. 中药材,2010,33(10):1651 YU XC,LIU GF.The response surface analysis method in the application of traditional Chinese medicine extraction and preparation technology[J].J Chin Med Mater,2010,33(10):1651
[10] MYERS RH.Response surface methodology current status and future directions[J].J Qual Technol,1999,31(1):30
[11] MENG FX,LI YX,GUO WL,et al.Optimization of fermentation medium for epothilones production with sequential statistical approach[J].Chem Res Chin Univ,2010,26(1):87
[12] 程玲铃,孙梅,涂凌.决明子提取物对植物病原菌的抑菌活性初探[J]. 四川理工学院学报,2005,18(2):53 CHENG LL,SUN M,TU L.The bacteriostatic activity of Cassia seed extract for plant pathogenic bacteria[J].J Sichuan Univ Sci Eng,2005,18(2):53
[13] 胡林峰,许明录,朱红霞. 植物精油抑菌活性研究进展[J]. 天然产物研究与开发,2011,23(2):384 HU LF,XU ML,ZHU HX.Advances in antifungal activity of plant essential oil[J].Nat Prod Res Dev,2011,23(2):384