黑胡椒挥发油β-环糊精包合物的制备及化学组分的GC-MS分析  

Preparation of β-Cyclodextrin Inclusion of Volatile Oil from Piperis Fructus and Analysis of Volatile Components by GC-MS

作　　者：盛琳[1,2] 周梦丽[2] 王勇[2] 尹蓉莉[1] 罗海燕[2] 

机构地区：[1]成都中医药大学药学院,成都611137 [2]海南医学院药学院,海口571199

出　　处：《中国实验方剂学杂志》2015年第9期4-9,共6页Chinese Journal of Experimental Traditional Medical Formulae

基　　金：海南省教育厅高校科研项目(Hjkj2012-34)

摘　　要：目的:建立黑胡椒挥发油的β-环糊精(β-CD)包合工艺,分析挥发油化学组分,为固化黑胡椒挥发油粉末的内在品质评价、制剂工艺及质量控制提供参考。方法:采用饱和水溶液法制备黑胡椒油β-CD包合物,以黑胡椒油与β-CD的配比、包合温度和包合时间为考察因素,包合物含油率、挥发油包合率和包合物收得率的综合评分为指标,通过均匀设计法优化制备工艺,经显微观察和热重分析进行包合物形成的验证,采用气相色谱-质谱联用技术(GC-MS)比较包合前后挥发油及经再次蒸馏原料油中组分的种类和含量。结果:最佳制备工艺为加6倍量β-CD于60℃包合4 h;包合物平均含油率11.56%,黑胡椒挥发油平均包合率75.32%,包合物平均收率86.13%。黑胡椒挥发油、包合物和经再次蒸馏的挥发油中分别鉴定出了46,40,45种化学成分,主要成分的构成基本一致,含量较高的6种成分总和占挥发油的70%以上;包合物和再次蒸馏后的黑胡椒挥发油新增和减失的成分比例均不到1%。结论:优选的包合工艺简便可行,可供黑胡椒油固化粉末的生产及质量控制参考。Objective： To establish a preparation technology of β-cyclodextrin （β-CD） inclusion of volatile oil from Piperis Fructus and to analysis of volatile components by GC-MS. Method： β-CD inclusion of volatile oil from Piperis Fructus was prepared by saturated aqueous solution method, with ratio of β-CD to volatile oil from Piperis Fructus, inclusion temperature and time as factors, comprehensive score of oil content in inclusion, inclusion rate of volatile oil and inclusion yield as index, inclusion conditions were optimized by uniform design. Inclusion was verified through microscopic examination and thermo-gravimetric analysis. GC-MS was employed to compare chemical compositions and percentages of samples which included volatile oil from Piperis Fructus, β-CD inclusion and redistilled volatile oil. Result： Optimum preparation conditions were as follows： β-CD to volatile oil ratio of 6： 1, inclusion time of 4 h, inclusion temperature at 60 ℃. Oil content in inclusion, inclusion rate of volatile oil and inclusion yield were 11.56% , 75.32% and 86.13% , respectively. These were 46, 40 and 45 chemical components were identified from volatile oil, /3-CD inclusion and redistilled volatile oil, respectively. But compositions in these samples were very similar, proportions of six main components in total contents of samples were more than 70%. There were some new chemicals appeared and some chemicals disappeared after inclusion and being redistilled, but the total content of these compounds was less than 1% , so that major components of each sample were almost the same. Conclusion： This inclusion process is simple andfeasible for production and quality evaluation of solidified powder of volatile oil from Piperis Fructus.

关 键 词：黑胡椒 挥发油 Β-环糊精 含油率 

分 类 号：R283.6[医药卫生—中药学] R284.1[医药卫生—中医学]