CN110082457A - A kind of detection method of Chinese prickly ash pericarp fragrance component - Google Patents
A kind of detection method of Chinese prickly ash pericarp fragrance component Download PDFInfo
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- CN110082457A CN110082457A CN201910457889.9A CN201910457889A CN110082457A CN 110082457 A CN110082457 A CN 110082457A CN 201910457889 A CN201910457889 A CN 201910457889A CN 110082457 A CN110082457 A CN 110082457A
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- China
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- prickly ash
- chinese prickly
- fragrance component
- detection method
- ash pericarp
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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
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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
Abstract
The present invention relates to a kind of detection methods of Chinese prickly ash pericarp fragrance component, first by Chinese prickly ash pericarp sample mill to be measured at powder, the Chinese prickly ash pericarp powder that constant weight is weighed after sieving is placed in ml headspace bottle, and ml headspace bottle is sealed with silica gel dottle pin, and the sample after fulling shake directly then is carried out GC-MS detection.The present invention is extracted and is analyzed to Chinese prickly ash fragrance component using headspace solid-phase microextraction combination low-polarity components, sample pre-treatments are not necessarily to solvent extraction, Environmental Safety, it is simple and quick, avoid cumbersome preprocessing process, and amount of samples is few, can intuitively reflect Chinese prickly ash pericarp fragrance component feature.
Description
Technical field
The present invention relates to technical field of analysis and detection, and in particular to a kind of to use headspace solid-phase microextraction combination gas chromatography mass spectrometry
Technology is extracted and the method for detection Chinese prickly ash pericarp fragrance component.
Background technique
The quality of Chinese prickly ash generally refers to the color, granular size, fragrance and fiber crops taste of Chinese prickly ash pericarp.Chinese prickly ash is as a kind of master
Flavouring is wanted, the fragrance of pericarp and numb taste are the important embodiments of Chinese prickly ash quality, and wherein fragrance is a weight for determining Chinese prickly ash quality
Factor is wanted, consumer's desire to purchase and commodity price are influenced.Therefore, there is great meaning to the research of Chinese prickly ash pericarp fragrance component
Justice, the analysis measurement of fragrance are always the important topic of Chinese prickly ash production and scientific research field.
Traditional test method is generally based on sensory evaluation, but sensory evaluation has subjectivity again can not be to fragrance component
Quantified, influences the accuracy of measurement result.Researcher is had been able to by modern comfort means to various Chinese prickly ash fruits
The various aroma substances such as alcohols, aldehydes, esters in skin are identified, wherein being exactly to carry out to it to the research first step of fragrance
Separation is extracted, it is directly related to the qualitative, quantitative of fragrance as a result, common Different Aroma Extraction Methods have Microwave-assisted Extraction water intaking to steam
Gas extraction, normal pressure and decompression water steam distillation, organic solvent extractionprocess and Simultaneous distillation, supercritical extraction
With head space adsorption etc., but since the Aromatic Matter Contents in Chinese prickly ash pericarp are extremely low, complicated components, high volatility are unstable,
The loss or conversion of substance are had in the extraction process of fragrance, and are easy to be influenced by external environment, the perfume (or spice) detected
Gas component and content are sufficiently complete reliable, and chemical extraction can also cause serious pollution to environment.
Therefore how to provide the simple and quick, efficient pollution-free of one kind and the accurate Chinese prickly ash pericarp fragrance component detection technique of result
It is those skilled in the art's urgent problem to be solved.
Summary of the invention
In view of this, can detect Chinese prickly ash fruit simultaneously the present invention provides a kind of detection technique used rapidly and efficiently
60 kinds or more of fragrance component in skin.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of detection method of Chinese prickly ash pericarp fragrance component, comprising the following steps:
(1) will be sieved after Chinese prickly ash pericarp sample comminution to be measured, obtain Chinese prickly ash fruit peel powder, weigh later a certain amount of powder by its
It is placed in ml headspace bottle, then seals ml headspace bottle and fullys shake；
(2) sample after fulling shake directly is subjected to GC-MS detection.
Preferably, 40 meshes are smashed it through in the step (1).
The beneficial effect of above-mentioned optimal technical scheme is: granularity is meticulous, and sample does not allow easy grinding and fragrance loss is serious, grain
Then the efficiency of Chinese prickly ash fragrance extraction is lower when spending big, chooses 40 mesh and following granularity is the simplicity of certifiable operation, and can
Ensure extraction efficiency.
Preferably, Chinese prickly ash fruit peel powder 0.05g~0.1g is weighed in the step (1) to be placed in 20mL ml headspace bottle.
The beneficial effect of above-mentioned optimal technical scheme is: when sample size is larger, being easy to keep chromatographic peak excessively high or even beyond conjunction
Range is managed, causes result inaccurate；Sample size is less compared with few fragrance for being then not easy to weigh and can extract, and will also result in result
Inaccuracy.
Preferably, ml headspace bottle is sealed using silica gel dottle pin in the step (1).
The beneficial effect of above-mentioned optimal technical scheme is: the temperature resistant range of silica gel Teflon combination is compared at 40~200 DEG C
It is suitable in General Purpose Rubber in harsh vapor detection environment.
Preferably, extracting head is 65 μm of PDMS/DVB materials, extraction preceding 230 in GC-MS detection process in the step (2)
DEG C activation 3min.
The beneficial effect of above-mentioned optimal technical scheme is: the substance of different extracting head type extractions is different, and PDMS/DVB is more
Be conducive to the extraction of volatile component.
Preferably, in the step (2) in GC-MS detection process extraction temperature be 50~80 DEG C, extraction time be 20~
60min。
The beneficial effect of above-mentioned optimal technical scheme is: low temperature extraction effect is poor, and temperature increases the extraction for being conducive to fragrance,
But when the temperature is excessively high, promotion effect is no longer significant and wastes energy, and extraction time is very few, and fragrance can not be extracted sufficiently, extends
Time will increase extraction efficiency, but overlong time increase effect is not significant and wastes energy, when by controlling reasonable extraction
Between and temperature, so that extraction efficiency and effect is reached best.
Preferably, 1~3min of desorption time in GC-MS detection process in the step (2).
The beneficial effect of above-mentioned optimal technical scheme is: desorption time is very few, and fragrance extraction is less, and the extension time will increase
Extraction efficiency, but overlong time increase effect is not significant and wastes energy.
Preferably, in step (2) the GC-MS detection, GC conditions are as follows:
Chromatographic column: TG-5MS quartz capillary column (30m × 0.25mm × 0.25 μm)；
Injector temperature: 250 DEG C；
Split ratio: 80:1；
Flow velocity: 80.0mL/min；
Pressure: 53kPa；
Sample volume: 1 μ L；
Program temperature:, keeping 2min by 50 DEG C of initial temperature, then with 3 DEG C/min temperature programming to 130 DEG C, keeps 2min,
200 DEG C are warming up to 4 DEG C/min again, keeps 2min, is then warming up to 230 DEG C with 20 DEG C/min, keeps 5min；
Carrier gas: the helium of purity >=99.999%；
Mass Spectrometry Conditions are as follows:
Ionization mode: EI；
Electron energy: 70eV；
Ion source temperature: 250 DEG C；
Interface temperature: 250 DEG C；
Scanning range: 50~550m/z；
ACQ mode: Scan；
Mass spectrogram is qualitative using NIST database combination document report auxiliary, and the guarantor of substance is determined using n-alkane as mark product
Index is stayed, bergamio is the content of aroma-producing substance in external standard semiquantitative determination Chinese prickly ash odor characteristics.
The beneficial effect of above-mentioned optimal technical scheme is: can be by different volatilizations by controlling suitable gas spectrum and Mass Spectrometry Conditions
Property ingredient separate, in order to detect identification.
In conclusion compared with prior art, the present invention has following technical effect that this method using the micro- extraction of head space solid phase
It takes and low-polarity components is combined to extract and analyze Chinese prickly ash pericarp fragrance component, sample pre-treatments are simple and quick, avoid
Cumbersome preprocessing process, and amount of samples is few；Sample is ground to direct injection analysis after shaking, avoids sample handling processes
In fragrance component loss, extract can reflect Chinese prickly ash pericarp odor characteristic well, especially suitable for some in Chinese prickly ash pericarp
The analysis of trace constituent, and be easy to carry out on-line checking；Determine that the retention index of substance is next qualitative using n-alkane as mark product
Fragrance component, the different influence to result of ingredient appearance time caused by avoiding because of experiment condition difference；Using acetic acid virtue
Camphor tree ester is external standard, and the method different from the past for determining fragrance component content with peak area normalization method has and utilizes different sample room ratios
Compared with component difference, on the whole, the detection method for the Chinese prickly ash fragrance component that the present invention establishes overcomes the deficiencies in the prior art,
Analytical technology is simple, quickly and no solvent residue, eliminate the solvent extraction of traditional extraction process elder generation sample introduction is analyzed again to fragrance at
The influence divided, the volatile matter of extraction can preferably reflect the original odor characteristic of Chinese prickly ash pericarp, be Chinese prickly ash pericarp fragrance component
Extracting and developing and analysis provide a kind of green, quickly and effectively method.
The bright book of attached drawing
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is influence diagram of the extraction temperature of the present invention to fragrance quantity；
Fig. 2 attached drawing is influence diagram of the extraction time of the present invention to fragrance quantity；
Fig. 3 attached drawing is influence diagram of the desorption time of the present invention to fragrance quantity；
Fig. 4 attached drawing is orthogonal experiments figure of the present invention；
Fig. 5 attached drawing is retest figure of the invention.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
The selection of optimum test condition:
Test parameters is taken to carry out single factor test orthogonal test, test process is as shown in table 1, as a result as shown in Fig. 4, passes through
Remaining parameter constant is controlled, changes extraction temperature, extraction time and desorption time, influence of the test variable to result, knot respectively
Fruit is as illustrated in the accompanying drawings from 1 to 3:
Optimal experimental condition is chosen by attached drawing 1-4, i.e. extracting head chooses PDMS/DVB, and 60 DEG C of extraction temperature, when extraction
Between 30min, 1~3min of desorption time.
Above-mentioned condition is taken specifically to be tested, process is as follows:
A kind of detection method of Chinese prickly ash pericarp fragrance component, comprising the following steps:
(1) 40 meshes will be crossed after Chinese prickly ash pericarp sample comminution to be measured, obtain Chinese prickly ash fruit peel powder, weigh the powder of 0.05g later
It places it in 20mL ml headspace bottle, ml headspace bottle is then sealed using silica gel dottle pin and fullys shake；
(2) sample after fulling shake directly is subjected to GC-MS detection.
Wherein, extracting head is 65 μm of PDMS/DVB materials in GC-MS detection process, extracts preceding 230 DEG C of activation 3min；Extraction
Temperature is 60 DEG C, extraction time 30min；Desorption time 1min.
In GC-MS detection process, GC conditions:
Chromatographic column: TG-5MS quartz capillary column (30m × 0.25mm × 0.25 μm)；
Injector temperature: 250 DEG C；
Split ratio: 80:1；
Flow velocity: 80.0mL/min；
Pressure: 53kPa；
Sample volume: 1 μ L；
Program temperature:, keeping 2min by 50 DEG C of initial temperature, then with 3 DEG C/min temperature programming to 130 DEG C, keeps 2min,
200 DEG C are warming up to 4 DEG C/min again, keeps 2min, is then warming up to 230 DEG C with 20 DEG C/min, keeps 5min；
Carrier gas: the helium of purity >=99.999%；
Mass Spectrometry Conditions:
Ionization mode: EI；
Electron energy: 70eV；
Ion source temperature: 250 DEG C；
Interface temperature: 250 DEG C；
Scanning range: 50~550m/z；
ACQ mode: Scan；
Mass spectrogram is qualitative using NIST database combination document report auxiliary, and the guarantor of substance is determined using n-alkane as mark product
Index is stayed, bergamio is the content of aroma-producing substance in external standard semiquantitative determination Chinese prickly ash odor characteristics.
The spectrogram of the Chinese prickly ash fragrance obtained by the method for embodiment 1 is as shown in Fig. 5, and repetitive operation 3 times, ingredient point
It is as shown in the table to analyse table:
Via attached drawing 5 and above table it is found that technical solution of the present invention can quickly and effectively measure Chinese prickly ash fragrance at
Point, application and popularization value with higher.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (8)
1. a kind of detection method of Chinese prickly ash pericarp fragrance component, which comprises the following steps:
(1) it will be sieved after Chinese prickly ash pericarp sample comminution to be measured, obtain Chinese prickly ash fruit peel powder, weigh a certain amount of powder later and place it in
In ml headspace bottle, then seals ml headspace bottle and fully shake；
(2) sample after fulling shake directly is subjected to GC-MS detection.
2. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(1) 40 meshes are smashed it through in.
3. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(1) Chinese prickly ash fruit peel powder 0.05g~0.1g is weighed in be placed in 20mL ml headspace bottle.
4. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(1) ml headspace bottle is sealed using silica gel dottle pin in.
5. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(2) extracting head is 65 μm of PDMS/DVB materials in GC-MS detection process in, extracts preceding 230 DEG C of activation 3min.
6. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(2) extraction temperature is 50~80 DEG C in GC-MS detection process in, and extraction time is 20~60min.
7. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(2) 1~3min of desorption time in GC-MS detection process in.
8. a kind of detection method of Chinese prickly ash pericarp fragrance component according to claim 1, which is characterized in that the step
(2) in GC-MS detection, GC conditions are as follows:
Chromatographic column: TG-5MS quartz capillary column (30m × 0.25mm × 0.25 μm)；
Injector temperature: 250 DEG C；
Split ratio: 80:1；
Flow velocity: 80.0mL/min；
Pressure: 53kPa；
Sample volume: 1 μ L；
Program temperature:, keeping 2min by 50 DEG C of initial temperature, then with 3 DEG C/min temperature programming to 130 DEG C, holding 2min, then with
4 DEG C/min is warming up to 200 DEG C, keeps 2min, is then warming up to 230 DEG C with 20 DEG C/min, keeps 5min；
Carrier gas: the helium of purity >=99.999%；
Mass Spectrometry Conditions are as follows:
Ionization mode: EI；
Electron energy: 70eV；
Ion source temperature: 250 DEG C；
Interface temperature: 250 DEG C；
Scanning range: 50~550m/z；
ACQ mode: Scan；
Mass spectrogram is qualitative using NIST database combination document report auxiliary, determines that the reservation of substance refers to using n-alkane as mark product
Number, bergamio are the content of aroma-producing substance in external standard semiquantitative determination Chinese prickly ash odor characteristics.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112083100A (en) * | 2020-09-11 | 2020-12-15 | 成都市食品药品检验研究院 | Method for simultaneously detecting multiple volatile components in pepper or pepper product |
| CN116338020A (en) * | 2022-10-26 | 2023-06-27 | 西北农林科技大学 | Method for detecting volatile terpenoid in pepper fruits and application thereof |
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Cited By (2)
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| CN112083100A (en) * | 2020-09-11 | 2020-12-15 | 成都市食品药品检验研究院 | Method for simultaneously detecting multiple volatile components in pepper or pepper product |
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