CN111157654A - Method for extracting and analyzing components of fraxinus chinensis leaf volatile oil - Google Patents
Method for extracting and analyzing components of fraxinus chinensis leaf volatile oil Download PDFInfo
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- CN111157654A CN111157654A CN202010034543.0A CN202010034543A CN111157654A CN 111157654 A CN111157654 A CN 111157654A CN 202010034543 A CN202010034543 A CN 202010034543A CN 111157654 A CN111157654 A CN 111157654A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention belongs to the technical field of traditional Chinese medicine extraction, detection and analysis, and particularly discloses a method for extracting and analyzing components of fraxinus chinensis leaf volatile oil, which comprises the following steps: s1, cleaning and crushing fresh Fraxinus chinensis leaves to obtain Fraxinus chinensis leaf crushed leaves; weighing 0.3-0.6g of crushed leaves of Fraxinus chinensis leaf, filling into a headspace bottle, and covering the bottle cap; s2, opening a headspace instrument, and performing headspace extraction at 80-90 ℃ for 20-40 min; s3, detecting by a GC-MS combined instrument; and S4, spectrogram retrieval. The extraction and analysis method adopts the headspace method and GC-MS to extract and analyze the volatile oil components in the leaf of Fraxinus chinensis, has the advantages of high extraction efficiency, simple operation, no solvent, mild conditions, short detection and analysis time, no damage to the chemical components of the leaf of Fraxinus chinensis, no loss of the most volatile compounds, and is an excellent method for researching the volatile oil components of the leaf of Fraxinus chinensis.
Description
Technical Field
The invention belongs to the technical field of extraction, detection and analysis of traditional Chinese medicines, and particularly relates to a method for extracting and analyzing components of fraxinus chinensis leaf volatile oil.
Background
The traditional Chinese medicine is precious wealth of Chinese nationality, has long history, wide application and unique characteristics. The success rate of developing new drugs by traditional Chinese medicine ethnic medicine is high, the potential is huge, and the prospect is wide. When the traditional Chinese medicine ethnic medicine is used for developing a new medicine, the effective substances in the traditional Chinese medicine ethnic medicine are often required to be extracted and separated.
White wool wax, another name: white wax with water. The plants belonging to the genus Paraffin, Cera chinensis and Ligustrum quihoui of Oleaceae can be used as the leaves of the medicine. According to the title of Shanxi Chinese herbal medicine, the water white wax has main functions: clearing away heat and toxic material. It is used to treat scald and trauma. Collected in summer and autumn, dried in the sun or fresh. Nature, flavor and meridian tropism: bitter and cool. According to the record of Sichuan common Chinese herbal medicine, shui Bai Chi has the main functions: clear heat and purge fire. It is used to treat hematemesis, toothache, aphtha, sore throat, and itching sore due to damp-heat and yellow water.
At present, no relevant literature report on the extraction analysis of the volatile oil component of the Chinese white wax leaves is found at home and abroad.
For samples containing volatile oils, steam distillation and organic solvent extraction are currently the most common methods, but both methods lose some volatile compounds, such as low molecular weight terpenes and small molecular esters.
Disclosure of Invention
The invention aims to provide a method for extracting and analyzing components of leaf volatile oil of Chinese white wax, which aims to solve the technical problem that volatile compounds are lost by a steam distillation method and an organic solvent method.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for extracting and analyzing components of leaf volatile oil of Fraxinus chinensis comprises the following steps:
s1, cleaning and crushing fresh Fraxinus chinensis leaves to obtain Fraxinus chinensis leaf crushed leaves; weighing 0.3-0.6g of crushed leaves of Fraxinus chinensis leaf, filling into a headspace bottle, and covering the bottle cap;
s2, opening a headspace instrument, and performing headspace extraction at 80-90 ℃ for 20-40 min;
s3, detecting by a GC-MS combined instrument;
(1) chromatographic conditions;
sample inlet temperature: 200 ℃ and 250 ℃;
heating the column to 200 ℃ and 250 ℃ at a heating rate of 5-10 ℃/min, and operating the whole heating process for 35-50 min;
the split ratio is 1-5: 1;
(2) mass spectrometry conditions;
the ionization mode is EI source; energy: 70 eV;
ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 280 ℃;
the mass range is 30-350 amu;
electron multiplier voltage: 1765V;
and S4, spectrogram retrieval.
Preferably, the initial temperature of the chromatographic column is 50-60 ℃, the temperature is raised to 150-160 ℃ at the temperature raising rate of 8 ℃/min after the initial temperature of the chromatographic column is maintained for 0.5-1.5min, and the temperature is raised to 200-250 ℃ at the temperature raising rate of 8 ℃/min after the initial temperature of the chromatographic column is maintained for 1-3 min; the operation is carried out for 35-50 min.
The beneficial effects of this technical scheme lie in:
(1) the extraction and analysis method adopts the headspace method and GC-MS to extract and analyze the volatile oil components in the leaf of the Fraxinus chinensis, has the advantages of high extraction efficiency, simple operation, no solvent, short time and mild conditions, does not damage the chemical components of the leaf of the Fraxinus chinensis, does not lose volatile compounds, and is an excellent method for researching the volatile oil components of the leaf of the Fraxinus chinensis.
(2) The extraction and analysis method comprises the steps of performing headspace extraction on volatile oil components of the Fraxinus chinensis, analyzing the components by using a GC-MS (gas chromatography-mass spectrometry) combined instrument, determining relative percentage content by using a peak area normalization method, and performing retrieval by using a CAS (CAS spectral library). The Fraxinus chinensis leaves are completely deformed under the condition, the matching degree of the generated peaks is high, impurity peaks do not exist, and the precision and the accuracy of the whole extraction analysis method are good.
(3) The extraction analysis method analyzes the volatile oil of the leaves of the Chinese white wax, identifies 11 compounds in the volatile oil components of the Chinese white wax, compares the compounds with the volatile oil components of the ligustrum quihoui, and detects the following components for the first time: leaf alcohol; cis-4-hexen-1-ol, 15-crown-5, wintergreen oil, n-hexanol, 3-hexen-1-ol, ethylvinyl methanol, geranial, 2-hexenal, cis-2-hexen-1-ol, 18-crown-6.
The method adopts a water vapor distillation method or an organic solvent method to detect no more components of the ligustrum quihoui under the same conditions, which fully proves that: the method analyzes the importance and novelty of the volatile oil of the leaves of the Chinese white wax, and can detect the medicinal components which are not contained in the ligustrum quihoui in the volatile oil of the leaves of the Chinese white wax.
(4) The extraction and analysis method is based on the unique medical theory of the multi-purpose fresh plant medicine of the national medicine, and has important significance for the research of medicinal basic substances of volatile oil components in the medicinal plant of the national medicine.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
A method for extracting and analyzing components of leaf volatile oil of Fraxinus chinensis comprises the following steps:
s1, cleaning and crushing fresh Fraxinus chinensis leaves to obtain Fraxinus chinensis leaf crushed leaves; weighing 0.3-0.6g of crushed leaves of Fraxinus chinensis leaf, filling into a headspace bottle, and covering the bottle cap;
s2, opening a headspace instrument, and performing headspace extraction at 80-90 ℃ for 20-40 min;
s3, detecting by a GC-MS combined instrument;
(1) chromatographic conditions;
sample inlet temperature: 200 ℃ and 250 ℃; under the condition that the split ratio is not changed, when the temperature of a sample inlet is lower than 200 ℃, the temperature of the sample inlet is too low, or when the temperature of the sample inlet is higher than 250 ℃, the problems of incomplete sample removal and low peak matching degree can occur;
the initial temperature of the chromatographic column is 50-60 ℃, the temperature is increased to 160 ℃ at the heating rate of 8 ℃/min after the initial temperature is maintained for 0.5-1.5min, the temperature is increased to 250 ℃ at the heating rate of 8 ℃/min after the initial temperature is maintained for 1-3min, and the temperature is maintained for about 10 min; the whole temperature rise process is carried out for 35-50 min; in the temperature rising process of the chromatographic column, the temperature rising time of the chromatographic column is strictly controlled, otherwise, the chromatographic separation time is prolonged, and even if the sample is completely lost and the peak matching degree is high, the problem that the impurity peak still exists is solved;
the split ratio is 1: 1;
(2) mass spectrometry conditions;
the ionization mode is EI source; energy: 70 eV;
ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 280 ℃;
the mass range is 30-350 amu;
electron multiplier voltage: 1765V;
and S4, spectrogram retrieval.
Example 1 the compounds analyzed by extraction, relative amounts and match data are given in table 1 below.
TABLE 1
Comparative example
Extracting volatile oil from fresh leaves of Fraxinus chinensis by steam distillation, analyzing chemical components by GCMS, and referring to Table 2 below for the extracted and analyzed components, relative contents and matching degree.
TABLE 2
And (4) conclusion:
the components extracted and analyzed in the comparative example are analyzed and compared with the components extracted and analyzed in the example 1, and the same components are only the same, so that the method fully proves that the extraction analysis method in the example has high extraction efficiency, simple and convenient operation, no solvent, short time and mild conditions, does not damage the chemical components of the leaf of the Fraxinus chinensis, does not lose volatile compounds, is an excellent method for researching the volatile oil components of the leaf of the Fraxinus chinensis, and has important significance for researching the medicinal basic substances of the volatile oil components in medicinal plants of national medicines.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (2)
1. The method for extracting and analyzing the components of the fraxinus chinensis leaf volatile oil is characterized by comprising the following steps:
s1, cleaning and crushing fresh Fraxinus chinensis leaves to obtain Fraxinus chinensis leaf crushed leaves; weighing 0.3-0.6g of crushed leaves of Fraxinus chinensis leaf, filling into a headspace bottle, and covering the bottle cap;
s2, opening a headspace instrument, and performing headspace extraction at 80-90 ℃ for 20-40 min;
s3, detecting by a GC-MS combined instrument;
(1) chromatographic conditions;
sample inlet temperature: 200 ℃ and 250 ℃;
heating the column to 200 ℃ and 250 ℃ at a heating rate of 5-10 ℃/min, and operating the whole heating process for 35-50 min;
the split ratio is 1-5: 1;
(2) mass spectrometry conditions;
the ionization mode is EI source; energy: 70 eV;
ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃; transmission line temperature: 280 ℃;
the mass range is 30-350 amu;
electron multiplier voltage: 1765V;
and S4, spectrogram retrieval.
2. The method for extracting and analyzing components of fraxinus chinensis leaf volatile oil according to claim 1, wherein the chromatographic conditions are as follows: the initial temperature of the chromatographic column is 50-60 ℃, the temperature is raised to 150-160 ℃ at the heating rate of 8 ℃/min after the initial temperature of the chromatographic column is maintained for 0.5-1.5min, and the temperature is raised to 200-250 ℃ at the heating rate of 8 ℃/min after the initial temperature of the chromatographic column is maintained for 1-3 min; the operation is carried out for 35-50 min.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150087520A1 (en) * | 2013-09-25 | 2015-03-26 | Agrofresh Inc. | Systems and methods for sovlent-free delivery of volatile compounds |
| CN106324120A (en) * | 2016-08-09 | 2017-01-11 | 西藏藏医学院 | Volatile component measuring method for Tibetan medicine heracleum millefolium diels |
-
2020
- 2020-01-14 CN CN202010034543.0A patent/CN111157654A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150087520A1 (en) * | 2013-09-25 | 2015-03-26 | Agrofresh Inc. | Systems and methods for sovlent-free delivery of volatile compounds |
| CN106324120A (en) * | 2016-08-09 | 2017-01-11 | 西藏藏医学院 | Volatile component measuring method for Tibetan medicine heracleum millefolium diels |
Non-Patent Citations (7)
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| 伍丹 等: "小蜡叶民间药用物质基础提取模式探索", 《教育教学论坛》 * |
| 宋秀华 等: "静态顶空与固相微萃取法测定元宝枫叶片挥发物成分比较", 《山东农业大学学报(自然科学版)》 * |
| 李彩芳 等: "SPME-GC-MS法分析小叶女贞挥发性化学成分", 《天然产物研究与开发》 * |
| 李玲 等: "运用GC-MS对三种不同方法提取的艾叶挥发油成分的比较分析", 《药学实践杂志》 * |
| 杨承清 等: "利用气质联用技术研究不同方法提取的黄心夜合鲜叶挥发油成分", 《南昌大学学报(理科版)》 * |
| 邱丽丽 等: "水蒸气蒸馏与顶空进样GC-MS分析白胡椒挥发性成分", 《食品科学》 * |
| 金华 等: "小叶水蜡树鲜花挥发油成分分析", 《安徽农业科学》 * |
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