CN111089929A - Gas chromatography-mass spectrometry combined analysis method for volatile oil of different processed products of immature bitter orange - Google Patents
Gas chromatography-mass spectrometry combined analysis method for volatile oil of different processed products of immature bitter orange Download PDFInfo
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- CN111089929A CN111089929A CN201911137978.1A CN201911137978A CN111089929A CN 111089929 A CN111089929 A CN 111089929A CN 201911137978 A CN201911137978 A CN 201911137978A CN 111089929 A CN111089929 A CN 111089929A
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- G—PHYSICS
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- 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
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- 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
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- 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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention provides a gas chromatography-mass spectrometry combined technique analysis method for volatile oil of different processed products of immature bitter orange, which relates to the field of traditional Chinese medicines and comprises the following steps: extracting volatile oil from fructus Aurantii Immaturus of different processed fructus Aurantii Immaturus products respectively and storing; establishing a gas chromatography-mass spectrometry combined technology analysis method to identify volatile oil components in different processed immature bitter orange products; and respectively identifying and recording components in different processed products of the immature bitter orange. According to the invention, through analysis of volatile oil components in different processed products of the immature bitter orange, experimental basis is provided for quality standard research of immature bitter orange decoction pieces, and more scientific and reasonable theoretical basis can be provided for clarifying processing mechanisms of the immature bitter orange decoction pieces by combining fingerprint spectrum research and pharmacodynamic research.
Description
Technical Field
The invention relates to the field of traditional Chinese medicines, in particular to a gas chromatography-mass spectrometry combined analysis method for volatile oil of different processed products of immature bitter orange.
Background
Immature bitter orange is bitter, pungent and sour in taste and slightly cold in nature, has the functions of breaking qi, removing food retention, resolving phlegm and dispersing distension and fullness, and is clinically often prepared into medicine in order to eliminate dryness and acidity. The Jiangxi zhangbang preparation method and the Jianchang bang preparation method are two important traditional side-making pies in China, and wheat bran and honey bran are respectively used as auxiliary materials to prepare medicinal materials. The related research of bran-fried immature bitter orange, the processing technology of immature bitter orange can be evaluated by mostly applying flavonoid chemical components, the related research on bran-fried volatile oil is less, and no report on unified comparative research on wheat bran processed products, honey bran processed products and raw products exists, but the research has positive guiding significance for explaining the processing mechanism and quality standard research of immature bitter orange.
Disclosure of Invention
The invention aims to provide a gas chromatography-mass spectrometry combined analysis method for volatile oil of different processed products of immature bitter orange, so as to solve the technical problems.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for analyzing volatile oil gas chromatography-mass spectrometry combined technology of different processed products of immature bitter orange comprises the following steps:
(1) extracting volatile oil from fructus Aurantii Immaturus of different processed fructus Aurantii Immaturus products respectively and storing;
(2) establishing a gas chromatography-mass spectrometry combined technology analysis method to identify volatile oil components in different processed immature bitter orange products;
(3) and respectively identifying and recording components in different processed products of the immature bitter orange.
Preferably, the processed products of different fructus aurantii immaturus conditions in the step (1) comprise raw fructus aurantii immaturus, bran-fried product, bran-fried honey product and bran-fried honey product.
Preferably, in the gas chromatography-mass spectrometry combined analysis in the step (2), the gas chromatography analysis conditions are that the sample port temperature is 260 ℃, the transmission line temperature is 250 ℃, the carrier gas is helium, the column flow rate is 1.0 mL/min < -1 >, the split ratio is 30: 1, the sample injection amount is 2 mu L, the temperature is programmed to rise, the column temperature is 70 ℃, and the temperature is raised to 150 ℃ at 2 ℃/min < -1 >; min-1 is raised to 186 ℃ at the temperature of 6 ℃; the temperature of 60 ℃ and min-1 is increased to 280 ℃ and kept for 1 min.
Preferably, the mass spectrometry conditions in the gas chromatography-mass spectrometry combination analysis are that an ionization mode adopts electron bombardment ionization, electron bombardment energy is 70eV, the ion source temperature is 230 ℃, the acceleration voltage is 34.6V, the resolution is 2500, the multiplier voltage is 1388V, the quadrupole rod temperature is 150 ℃, the scanning range is m/z 40-350, and the scanning times are 4.45 times/s.
Preferably, in the step (3), the mass spectrogram is subjected to computer data processing and NST11L and WILEY275 standard mass spectrogram library retrieval to identify various chemical components, and the relative mass fraction of each component in the sample is determined by a peak area normalization method.
The invention has the beneficial effects that:
in the invention, the wheat bran and the rice bran have the influence on the traditional Chinese medicine in that the auxiliary materials and other factors (such as heating) in the processing process play a comprehensive role together, so that the medicinal materials are changed in a series of chemical components, and the curative effect of the medicinal materials is further influenced. Immature bitter orange is good at moving qi and relieving distension, while stir-baked with bran is mild in action and good at regulating qi and strengthening spleen. The honey is a liquid auxiliary material commonly used in the processing of traditional Chinese medicines, and the honey-processed traditional Chinese medicines can enhance the functions of the medicines in relieving cough, moistening lung, tonifying spleen and benefiting qi. By analyzing the volatile oil components in different processed products of the immature bitter orange, an experimental basis is provided for the research on the quality standard of the immature bitter orange decoction pieces, and a more scientific and reasonable theoretical basis can be provided for the explanation on the processing mechanism of the immature bitter orange decoction pieces by combining the research on the fingerprint spectrum and the pharmacodynamics.
Detailed Description
The present invention will be further described with reference to specific embodiments for the purpose of facilitating an understanding of technical means, characteristics of creation, objectives and functions realized by the present invention, but the following embodiments are only preferred embodiments of the present invention, and are not intended to be exhaustive. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
Examples
A method for analyzing volatile oil gas chromatography-mass spectrometry combined technology of different processed products of immature bitter orange comprises the following steps:
(1) extracting volatile oil from fructus Aurantii Immaturus of different processed fructus Aurantii Immaturus products respectively and storing;
(2) establishing a gas chromatography-mass spectrometry combined technology analysis method to identify volatile oil components in different processed immature bitter orange products;
(3) and respectively identifying and recording components in different processed products of the immature bitter orange.
The different processed products of immature bitter orange in the step (1) comprise raw immature bitter orange, bran-fried products, honey bran-fried products and honey bran-fried products.
In the gas chromatography-mass spectrometry combined analysis in the step (2), the gas chromatography analysis conditions are that the sample port temperature is 260 ℃, the transmission line temperature is 250 ℃, the carrier gas is helium, the column flow rate is 1.0 mL/min < -1 >, the split ratio is 30: 1, the sample injection amount is 2 mu L, the temperature is programmed to rise, the column temperature is 70 ℃, and the temperature is raised to 150 ℃ at 2 ℃ min < -1 >; min-1 is raised to 186 ℃ at the temperature of 6 ℃; the temperature of 60 ℃ and min-1 is increased to 280 ℃ and kept for 1 min.
The mass spectrometry conditions in the gas chromatography-mass spectrometry combined analysis are that an ionization mode adopts electron bombardment ionization, the electron bombardment energy is 70eV, the ion source temperature is 230 ℃, the acceleration voltage is 34.6V, the resolution is 2500, the multiplier voltage is 1388V, the quadrupole rod temperature is 150 ℃, the scanning range is m/z 40-350, and the scanning frequency is 4.45 times/s.
In the step (3), the mass spectrogram is subjected to computer data processing and NST11L and WILEY275 standard mass spectrogram library retrieval to identify various chemical components, and the relative mass fraction of each component in the sample is determined by using a peak area normalization method.
The gas chromatography-mass spectrometry combined analysis shows that the types and content of volatile oil components in 4 immature bitter orange decoction pieces are obviously changed, the components which are identified after heating and processing are more than raw products, wherein 99 immature bitter oranges are identified by bran, 87 immature bitter oranges are identified by honey bran, 81 immature bitter oranges are identified by honey bran, and 79 raw immature bitter oranges are identified. The four ingredients share 42 volatile oil components. Compared with immature bitter orange, 52 compounds are added after stir-frying with bran, 26 compounds are added after stir-frying with honey bran, and 28 compounds are added after stir-frying with honey bran. And the content of partial compounds is increased or reduced. No 14 compounds in the immature bitter orange raw product are detected in each processed product, which indicates that component transformation possibly occurs in the processing process, such as the generation of the geraniol and the disappearance of the carveol in each processed product. The content of the main component limonene in the immature bitter orange volatile oil is small in different processed products, wherein the content of the immature bitter oranges stir-fried with bran is the highest (46.33%), and the content of the stir-fried honey bran is the lowest (40.89%). The content of gamma-terpinene after bran-frying is greatly reduced to only 2.66 percent, and the contents of the other three immature bitter orange decoction pieces are similar to each other and are about 9 percent. Because the dosage of the wheat bran, the honey bran and the honey bran is less in the processing process, the volatile oil component of the auxiliary materials has less influence on the processed product of the immature bitter orange. The results suggest that heating or interaction with excipients during processing may be the key factor in the change of volatile oil content and variety.
In the present invention, unless otherwise expressly stated or limited, "above" or "below" a first feature means that the first and second features are in direct contact, or that the first and second features are not in direct contact but are in contact with each other via another feature therebetween. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A method for analyzing volatile oil gas chromatography-mass spectrometry combined technology of different processed products of immature bitter orange is characterized by comprising the following steps: the method comprises the following steps:
(1) extracting volatile oil from fructus Aurantii Immaturus of different processed fructus Aurantii Immaturus products respectively and storing;
(2) establishing a gas chromatography-mass spectrometry combined technology analysis method to identify volatile oil components in different processed immature bitter orange products;
(3) and respectively identifying and recording components in different processed products of the immature bitter orange.
2. The gas chromatography-mass spectrometry combined analysis method for the volatile oil of different processed products of immature bitter orange according to claim 1, is characterized in that: the processed products of different fructus aurantii immaturus conditions in the step (1) comprise raw fructus aurantii immaturus, bran-fried products, honey bran-fried products and honey bran-fried products.
3. The gas chromatography-mass spectrometry combined analysis method for the volatile oil of different processed products of immature bitter orange according to claim 1, is characterized in that: in the gas chromatography-mass spectrometry combined analysis in the step (2), the gas chromatography analysis conditions are that the sample port temperature is 260 ℃, the transmission line temperature is 250 ℃, the carrier gas is helium, the column flow rate is 1.0 mL/min < -1 >, the split ratio is 30: 1, the sample injection amount is 2 mu L, the temperature is programmed to rise, the column temperature is 70 ℃, and the temperature is raised to 150 ℃ at 2 ℃ min < -1 >; min-1 is raised to 186 ℃ at the temperature of 6 ℃; the temperature of 60 ℃ and min-1 is increased to 280 ℃ and kept for 1 min.
4. The gas chromatography-mass spectrometry combined analysis method for the volatile oil of different processed products of immature bitter orange according to claim 3, wherein the gas chromatography-mass spectrometry combined analysis method comprises the following steps: the mass spectrometry conditions in the gas chromatography-mass spectrometry combined analysis are that an ionization mode adopts electron bombardment ionization, the electron bombardment energy is 70eV, the ion source temperature is 230 ℃, the acceleration voltage is 34.6V, the resolution is 2500, the multiplier voltage is 1388V, the quadrupole rod temperature is 150 ℃, the scanning range is m/z 40-350, and the scanning frequency is 4.45 times/s.
5. The gas chromatography-mass spectrometry combined analysis method for the volatile oil of different processed products of immature bitter orange according to claim 1, is characterized in that: in the step (3), the mass spectrogram is subjected to computer data processing and NST11L and WILEY275 standard mass spectrogram library retrieval to identify various chemical components, and the relative mass fraction of each component in the sample is determined by using a peak area normalization method.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650326A (en) * | 2020-07-03 | 2020-09-11 | 湖南旻一生物科技有限公司 | Quality control method and quality control spectrogram of volatile oil component of Chinese medicinal sachet, and construction method thereof |
| CN115236212A (en) * | 2021-04-22 | 2022-10-25 | 中国科学院上海药物研究所 | Quality detection method of euphorbia Chinese herbal medicine |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650326A (en) * | 2020-07-03 | 2020-09-11 | 湖南旻一生物科技有限公司 | Quality control method and quality control spectrogram of volatile oil component of Chinese medicinal sachet, and construction method thereof |
| CN115236212A (en) * | 2021-04-22 | 2022-10-25 | 中国科学院上海药物研究所 | Quality detection method of euphorbia Chinese herbal medicine |
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