回药方剂回回脑梗通挥发油的超临界CO2流体萃取工艺优化及其成分分析
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篇名: 回药方剂回回脑梗通挥发油的超临界CO2流体萃取工艺优化及其成分分析
TITLE:
摘要: 目的:优化治疗脑卒中的回药方剂回回脑梗通挥发油的超临界CO2流体萃取工艺,并对挥发油的成分进行分析鉴定。方法:以挥发油得率和肉桂醛含量为指标,以萃取压力、萃取温度和萃取时间为因素设计单因素试验和正交试验,并对优化后工艺进行验证试验;测定挥发油的理化指标;采用气相色谱-质谱法(GC-MS)并结合保留指数分析挥发油成分,以面积归一化法计算各成分的相对百分含量。结果:最优萃取工艺为萃取压力30 MPa、萃取温度50 ℃、萃取时间100 min;验证试验中挥发油得率为4.8%(RSD=0.02%,n=3)、肉桂醛含量为2.0 mg/g(RSD=1.8%,n=3);挥发油的相对密度为1.05、折光率为1.52、酸值为28.13 mg(KOH)/g、碘值为74.47 g(I)/100 g、皂化值为54.20 mg(KOH)/g、过氧化值为19.42 meq/kg;GC-MS分析结果表明挥发油成分与文献保留指数相似度在80%以上的化合物共31个,其中鉴定了21个,占总挥发油的44%,已鉴定的化合物中相对百分含量较高的有反式肉桂醛(9.14%)、β-石竹烯(3.21%)、α-没药醇(3.11%)、β-没药烯(2.56%)等。结论:优化的萃取工艺稳定可行;本试验所得萃取工艺和成分分析结果可为该方的开发利用提供试验基础和参考依据。
ABSTRACT: OBJECTIVE: To optimize supercritical CO2 fluid extraction (SFE-CO2) technology of volatile oil from Hui medicine Huihui Naogengtong for stroke, and to analyze and identify its component. METHODS: With yield of volatile oil and the content of cinnamaldehydeas indexes, and extraction pressure, temperature and time as factors, single factor test and orthogonal test were designed to optimize SFE-CO2 technology; optimized technology was also validated. Physical and chemical indexes of volatile oil were determined, and the constituents of volatile oil were analyzed by GC-MS and retention index. Relative percentage contents of each component were calculated by area normalization method. RESULTS: Optimal technology was as follows as extraction pressure 30 MPa, extraction temperature 50 ℃ and extraction time 100 min. In verification test, the yield of volatile oil was 4.8% (RSD=0.02%, n=3), and the content of cinnamylaldehyde was 2.0 mg/g (RSD=1.8%, n=3). Physicochemical properties of volatile oil were as follows as relative density 1.05, refractive index 1.52, acid value 28.128 mg(KOH)/g, iodine value 74.47       g(I)/100 g, saponification value 54.2 mg(KOH)/g, peroxide 19.42 meq/kg. GC-MS analysis showed the similarity with retention index in literatures of 31 compounds were more than 80%, 21 of them were identified and accounted for 44% of total volatile oil, among which E-cinnamaldehyde (9.14%), β-caryophyllene (3.21%), α-bisabolol (3.11%) and β-bisabolene (2.56%) had high relative percentage content. CONCLUSIONS: Optimal extraction technology is stable and feasible. The results of extraction technology and component analysis can provide important trail base and reference data for the exploration and utilization of Huihui Naogengtong.
期刊: 2016年第27卷第19期
作者: 管恩爽,张万年,张霞,李佼宁,陈丽,张立明
AUTHORS: GUAN Enshuang,ZHANG Wannian,ZHANG Xia,LI Jiaoning,CHEN Li,ZHANG Liming
关键字: 回药方剂;回回脑梗通;挥发油;正交试验;超临界CO2流体萃取工艺;肉桂醛含量;GC-MS;成分分析
KEYWORDS: Hui medicine; Huihui Naogengtong; Volatile oil; Orthogonal test; Supercritical CO2 fluid extraction technology; Cinnamylaldehyde content; GC-MS; Component analysis
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