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河南中医药大学 药学院,河南省中药资源与中药化学重点实验室,郑州 450046
薛淑娟,博士,讲师,从事中药质量标准研究,E-mail:sjxue3901@163.com
陈随清,博士,教授,从事中药品种整理与质量评价研究,Tel:0371-65676686,E-mail:suiqingchen0371@163.com
收稿日期:2021-07-02,
网络出版日期:2021-09-03,
纸质出版日期:2022-08-05
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薛淑娟,杨江凯,陈随清.GC-MS结合保留指数法解析太行菊挥发油的化学成分[J].中国实验方剂学杂志,2022,28(15):120-128.
XUE Shujuan,YANG Jiangkai,CHEN Suiqing.Analysis of Chemical Constitutions of Volatile Oil in Opisthopappus taihangensis by GC-MS Combined with Retention Index[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(15):120-128.
薛淑娟,杨江凯,陈随清.GC-MS结合保留指数法解析太行菊挥发油的化学成分[J].中国实验方剂学杂志,2022,28(15):120-128. DOI: 10.13422/j.cnki.syfjx.20211864.
XUE Shujuan,YANG Jiangkai,CHEN Suiqing.Analysis of Chemical Constitutions of Volatile Oil in Opisthopappus taihangensis by GC-MS Combined with Retention Index[J].Chinese Journal of Experimental Traditional Medical Formulae,2022,28(15):120-128. DOI: 10.13422/j.cnki.syfjx.20211864.
目的
2
研究太行菊挥发油的成分组成,为该药材的综合开发提供参考依据。
方法
2
以小白菊、小黄菊和野菊花作为对照,采用气相色谱-质谱法(GC-MS)结合保留指数法对太行菊及3个对照菊花品种的挥发油进行定性及定量分析,GC条件为程序升温(初始温度60 ℃,保持2 min;以5 ℃·min
-1
升温至120 ℃,保持2 min;以2 ℃·min
-1
升温至180 ℃,保持3 min;以8 ℃·min
-1
升温至240 ℃,保持5 min;以10 ℃·min
-1
升温至280 ℃,保持5 min),载气为高纯度氦气,分流比50∶1;MS条件为电子轰击离子源(EI),离子源温度230 ℃,电子碰撞能量70 eV,检测范围
m
/
z
30~445。采用主成分分析(PCA)和正交偏最小二乘法-判别分析(OPLS-DA)筛选太行菊与3个对照菊花品种中挥发油的差异性成分,明确其特征性。
结果
2
分别从太行菊、小白菊、小黄菊和野菊花的挥发油中鉴定出了86、96、112、109个化合物,其中四者共有成分73个。太行菊与对照菊花品种的挥发油含量差异较大,其中太行菊中
α
-侧柏酮、桉油精和4-松油烯醇的相对含量较高;而对照菊花品种中樟脑、桉油精和
α
-乙酸松油酯的相对含量均较高。PCA和OPLS-DA分析共筛选出11个化合物作为区分太行菊和3个对照菊花品种的特征性成分,其主要差异成分为兰香油薁和
δ
-杜松烯。
结论
2
太行菊挥发油主要含醇类、萜烯类、酮类及酯类成分,药用价值较高;GC-MS结合保留指数法可提高挥发油定性分析的准确性,可为太行菊的开发与利用提供参考。
Objective
2
To study the composition of volatile oil in
Opisthopappus taihangensis
(Taihangju), and provide a reference for comprehensive development of this medicine.
Method
2
Taking
Chrysanthemum morifolium
(Xiaobaiju),
C. morifolium
(Xiaohuangju) and
C. indicum
(Yejuhua) as control, the qualitative and quantitative analysis of volatile oil in Taihangju and three control varieties were completed by gas chromatography-mass spectrometry (GC-MS) combined with retention index method. The GC conditions were as following:programmed temperature (initial temperature at 60 ℃, kept for 2 min; up to 120 ℃ with the heating rate of 5 ℃·min
-1
, still kept for 2 min; up to 180 ℃ with the heating rate of 2 ℃·min
-1
, kept for 3 min; and then up to 240 ℃ with the heating rate of 8 ℃·min
-1
, kept for 5 min; finally up to 280 ℃ with the heating rate of 10 ℃·min
-1
,
kept it for 5 min and finished), high-purity helium as the carrier gas, the split ratio of 50∶1. MS conditions were as follows:electron impact ion source (EI), ion source temperature of 230 ℃, electron collision energy of 70 eV and scanning range of
m
/
z
30-445. Principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were used to obtain the characteristic components between Taihangju and the three control varieties.
Result
2
A total of 86, 96, 112 and 109 compounds including 73 common components were identified in Taihangju, Xiaobaiju, Xiaohuangju and Yejuhua, respectively. The contents of volatile components in Taihangju were significantly different from that of the control varieties. In which, the relative contents of
α
-thujone, eucalyptol and terpinen-4-ol were high in Taihangju, and eucalyptol, camphor and
α
-terpinyl acetate were the main compositions in the control varieties. In addition, 11 compounds were screened as characteristic components to distinguish Taihangju and the three control varieties by PCA and OPLS-DA, including main differential components of chamazulene and
δ
-cadinene.
Conclusion
2
The main components of volatile oil in Taihangju includes alcohols, terpenes, ketones and esters with high medicinal value. The accuracy of qualitative analysis of volatile oil is improved by GC-MS combined with retention index method, which provides scientific reference for development and utilization of Taihangju.
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