不同提取方式的枳术丸挥发油化学成分组成和含量对比分析  

Comparative analysis of chemical constituents and contents in volatile oil of Zhizhu pills extracted by different methods

作　　者：杜智勇[1] 宋志前[1] 王淳[1] 董运茁 宁张弛 刘元艳[2] 刘振丽[1] 

机构地区：[1]中国中医科学院中医基础理论研究所,北京100700 [2]北京中医药大学中药学院,北京100102

出　　处：《药物分析杂志》2015年第1期34-40,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：中央级公益性科研院所基本科研业务费专项资金资助[YZ-1317]

摘　　要：目的：k研究提取方式对枳术丸挥发油化学成分组成和含量的影响,为复方物质基础研究提供参考。方法：采用水蒸气蒸馏法提取枳术丸挥发油,挥发油提取器分别采用不包裹（见光）及用黑布包裹（避光）提取相同时间,分别得到见光与避光提取的挥发油。利用GC-MS联用技术进行成分分析。气相色谱条件：采用Rrestek-5MS石英毛细管柱（30 m×0.25 mm×0.25μm）,进样口温度250℃,程序升温（起始温度0℃,保持1 min,以5℃·min^-1升温至130℃,保持1 min,再以10℃·min^-1升温至240℃,保持1 min）,进样量1μL,载气为氦气,分流比为1∶30;质谱分析条件：电离方式为EI,离子源温度200℃,接口温度为250℃,电子能量70 e V,电离电压1.760 k V,质量扫描范围m/z 45-450 amu,溶剂切割时间3.5 min。通过质谱数据库检索和经对照品对照,确定成分结构,色谱峰峰面积归一化法计算各成分的相对百分含量。同时与炒白术、炒枳实挥发油进行对比,确定枳术丸挥发油化学成分来源。结果：避光与见光枳术丸挥发油得率分别为1.05%和1.03%,分别鉴定了54个和60个成分,成分种类主要为萜烯类,还有醇类、酸类、酯类等,但每种类型成分的个数不同;共有的成分46个,但各成分相对含量不同;含量高于1.0%的成分分别有10个和18个,它们的总量分别占挥发油总量的82.96%和76.17%;含量最高的成分都是柠檬烯,苍术酮含量差异最大。见光挥发油与避光挥发油相比,消失了8个成分,增加了13个成分。化学成分组成和含量变化显示,与避光挥发油比较,见光的枳术丸挥发油成分变化主要来自炒白术中成分的变化。结论：见光与避光提取的枳术丸挥发油得率没有明显差异,但化学成分组成和含量都发生了变化,尤其炒白术中成分见光不稳定。提示应关注实验过程可能引起的成分变化。Objective： To research the effects of different extraction methods on the chemical constituents and contents of volatile oil of Zhizhu pills,to provide a reference for studies of substance basis of Chinese compound prescription. Methods： The volatile oil of Zhizhu pills was extracted by steam distillation using two methods. In one method,the extractor was wrapped with black cloth to keep the oil out of the sun light（ dark condition oil）,while in the other method,the extractor was not wrapped so that the oil was exposed to the sun light（ light condition oil）. The volatile oil which obtained by the two methods were analyzed by GC-MS. GC conditions were as follows. A Rrestek-5MS capillary column（ 30 m × 0. 25 mm × 0. 25 μm） was adopted with the inlet temperature of 250 ℃ under the following heating program. The initial temperature was 0 ℃,kept for 1 min,with 5 ℃ ·min^-1 heating to130 ℃,kept for 1 min,then 10 ℃ ·min^-1 heating to 240 ℃,kept for 1 min. The injection volume was 1 μL,the carrier gas was helium,and the split ratio was 1∶ 30. MS analysis conditions were as follows. Ionization mode was EI,the ion source temperature was 200 ℃,the interface temperature was 250 ℃,the electron energy was 70 e V,the ionization voltage was 1. 760 k V and the mass scan range（ m / z） was 45-450 amu,the solvent cut time was3. 5 min. Then,the chemical constitutes of volatile oil were identified by data base retrieval and by comparing with mass spectrum data of the reference substance,and the relative amount of each constitute was calculated by area normalization method. Meanwhile,the fried Atractylodes macrocephala Koidz.（ Chao Baizhu） and the fried Citrus aurantium L.（ Chao Zhishi） volatile oils were adopted for comparison to determine the sources of chemical constitutes in Zhizhu volatile oil. Results： The yields of volatile oil extracted in dark and light conditions were 1. 05% and1. 03%,and fifty-four constitutes and sixty constitutes were identified in both conditions respec

关 键 词：枳术丸 白术 枳实 挥发油 避光提取 见光提取 气相色谱-质谱分析 

分 类 号：R917[医药卫生—药物分析学]