CN107621513A - A kind of adulterated discrimination method of natural rose essential - Google Patents
A kind of adulterated discrimination method of natural rose essential Download PDFInfo
- Publication number
- CN107621513A CN107621513A CN201711072489.3A CN201711072489A CN107621513A CN 107621513 A CN107621513 A CN 107621513A CN 201711072489 A CN201711072489 A CN 201711072489A CN 107621513 A CN107621513 A CN 107621513A
- Authority
- CN
- China
- Prior art keywords
- rose essential
- sample
- adulterated
- discrimination method
- natural rose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
A kind of adulterated discrimination method of natural rose essential, is related to Rosa Damascana.Take natural rose essential to be dissolved in absolute ethyl alcohol, after shaking up, draw 1mL injection sample bottles, then be positioned in injector；Enter menu editing from computer for analysis interface, editor, which finishes, presses " preservation " button；Set chromatographic quantitative analysis parameter；Set mass spectrometry analysis condition；Setting completed for chromatographic quantitative analysis parameter and mass spectrometry analysis condition, after baseline stability, click on " RUN ", gas chromatograph-mass spectrometer then starts automatical analysis detection, automatic sampler starts sample introduction, after the completion of sample introduction, sample introduction needle is rinsed using acetone, until the residual sample in sample introduction needle cleans up completely, analysis is completed by gas chromatograph-mass spectrometer, chromatographic quantitative analysis is directly read using area normalization method at gas chromatograph-mass spectrometer interface, and mass spectrometry analysis differentiates in gas chromatograph-mass spectrometer to the composition at each peak, therefrom chooses adulterated component substances.
Description
Technical field
The present invention relates to Rosa Damascana, more particularly, to a kind of adulterated discrimination method of natural rose essential.
Background technology
Rosa Damascana is the rare advanced concentration essence in the world, is the fine work in essential oil, is the advanced rare perfume of manufacture
Not only important but also expensive raw material, be not only used for manufacturing the cosmetics such as beauty, skin care, hair care, be also widely used in medical and food；
Rosa Damascana is one of most expensive essential oil in the whole world, a feast for the eyes adulterated essential oil of in the market, how to differentiate, seems particularly heavy
Will.
Chinese patent CN105938129A discloses a kind of GC chromatogram analysis methods of Ping Yin Rose essential oil, by Ping Yin Rose essence
Oil is dissolved in n-hexane, injects gas chromatograph, and gas chromatographic detection condition is as follows：Chromatographic column：HP INNOWax elastic capillaries
Tubing string, 250 DEG C of injector temperature, 250 DEG C of detector temperature；Carrier gas is nitrogen, flow velocity 0.5ml/min, split ratio 100：1.
Temperature programming：80 DEG C of initial temperature, 5min is kept, rise to 220 DEG C with 2 DEG C/min speed, keep 20min, the μ L of sample size 0.2.
Citronellol appearance time is 47.917min, and nerol appearance time is 49.653min, and geraniol appearance time is
52.061min；After instrument stabilizer, the content of main component in Ping Yin Rose essential oil is calculated.
Chinese patent CN104391054A discloses the GC/MS fingerprint images that a kind of and field Damask Rose essential oil is used for standard
Spectrum detection method；Using spectrogram similarity as evaluation index, from macroscopically control and field Damask Rose essential oil quality, really
The content range of its fixed property material, including head perfume, body note, bottom note, fixative ingredients and not existing standard is paid close attention to
Body note composition, the more fully overall fragrance of control and field Damask Rose essential oil, have paid close attention to high straight chain alkane
Composition and content, essential oil congealing point is effectively controlled, chemically more intuitively control outward appearance and fragrance on composition, formulate on this basis
The standard of property material quality testing, so as to substantially increase accuracy of detection and detection efficiency, available for field Damascus
The quality evaluation of Rosa Damascana, a kind of quality standard is provided for the quality control with field Damask Rose essential oil.
The content of the invention
It is an object of the invention to provide being mixed into for adulterated essential oil can be prevented, ensure one kind of essence and essential oil product quality
The adulterated discrimination method of natural rose essential.
The present invention comprises the following steps：
1) take natural rose essential to be dissolved in absolute ethyl alcohol, after shaking up, draw 1mL injection sample bottles, then be positioned over sample introduction
In device；
In step 1), the absolute ethyl alcohol can use the absolute ethyl alcohol for analyzing pure content 99.7%；The sample bottle can
Using 2mL automatic sampler sample bottles；The injector can be analyzed using automatic sampler, and sample size can be 1 μ L；It is described
Automatic sampler can use 16 liquid automatic samplers of 7693A Autoinjector.
2) menu editing is entered from computer for analysis interface, editor, which finishes, presses " preservation " button；
In step 2), the content of edit into menu editing include but is not limited to sample ID, model, lot number and
Sample is placed in space number corresponding to injector.
3) chromatographic quantitative analysis parameter is set；
In step 3), the chromatographic quantitative analysis parameter can be：
Chromatographic column：HP-5MS posts (60m × 0.25mm × 0.25 μm), FID flame ionization ditectors, carrier gas are helium
Gas, constant current mode, flow are 1.0~2.0ml/min, are not shunted；Temperature programming：80 DEG C of initial temperature, is warming up to 4 DEG C/min
280 DEG C, 5min is kept, rear operation is warming up to 300 DEG C, keeps 5min；Total run time 60min, 280 DEG C of satellite interface temperature.
4) mass spectrometry analysis condition is set；
In step 4), the mass spectrometry analysis condition can be：
230 DEG C of ion source temperature, 150 DEG C of quadrupole rod temperature, ionize mode EI, electron energy 70eV, the μ of heater current 34.6
A, the μ of quality of scanning scope 35~450.
5) setting completed for chromatographic quantitative analysis parameter and mass spectrometry analysis condition, after baseline stability, clicks on " RUN ",
Gas chromatograph-mass spectrometer then starts automatical analysis detection, and automatic sampler starts sample introduction, after the completion of sample introduction, using acetone to sample introduction needle
Rinsed, until the residual sample in sample introduction needle cleans up completely, analyze and completed by gas chromatograph-mass spectrometer, chromatographic quantitative analysis
Using area normalization method directly gas chromatograph-mass spectrometer interface read, mass spectrometry analysis in gas chromatograph-mass spectrometer to each peak into
Divide and differentiated, therefrom choose adulterated component substances.
In step 5), the gas chromatograph-mass spectrometer can use U.S. Agilent gas chromatograph-mass spectrometer Agilent 6890N-
5973I；The automatic sampler can use 16 liquid automatic samplers of Agilent 7693A Autoinjector；Described third
Ketone, which can use, analyzes pure, content 99.5%, and acetone is used for the automatic cleaning of sample introduction needle after the completion of sample introduction, belongs to cleaning agent；It is described
Rinsing to use at least 2 times.
The present invention can carry out GCMS calibratings to the natural rose essential purchased, and prevent being mixed into for adulterated essential oil, ensure fragrant
The quality of essence and essential oil product；Main component and content in Rosa Damascana can be quickly and accurately detected, effectively rejects adulterated essence
Oil, and method is simple, practicality, high sensitivity, stability is good, testing cost is low.
Brief description of the drawings
Fig. 1 is the rear signal result of the embodiment of the present invention.
Embodiment
The present invention is further illustrated for following examples.
The present invention comprises the following steps：
1) take natural rose essential to be dissolved in absolute ethyl alcohol, after shaking up, draw 1mL injection sample bottles, then be positioned over sample introduction
In device；The injector can be analyzed using automatic sampler, and sample size can be 1 μ L；The automatic sampler can use peace
Prompt 16 liquid automatic samplers of human relations 7693A Autoinjector；The sample bottle can use 2mL automatic sampler samples
Bottle.The absolute ethyl alcohol can use the absolute ethyl alcohol for analyzing pure content 99.7%.
2) menu editing is entered from computer for analysis interface, including but not limited to sample ID, model, lot number and sample is put
In space number corresponding to injector, editor, which finishes, presses " preservation " button；
3) chromatographic quantitative analysis parameter is set：Chromatographic column：HP-5MS posts (60m × 0.25mm × 0.25 μm), FID hydrogen flames
Ionization detector, carrier gas are helium, and constant current mode, flow is 1.0~2.0ml/min, is not shunted；Temperature programming：Initial temperature
80 DEG C of degree, 280 DEG C are warming up to 4 DEG C/min, keep 5min, rear operation is warming up to 300 DEG C, keeps 5min；Total run time
60min, 280 DEG C of satellite interface temperature；
4) mass spectrometry analysis condition is set：230 DEG C of ion source temperature, 150 DEG C of quadrupole rod temperature, ionize mode EI, electricity
Sub- energy 70eV, heater current 34.6 μ A, the μ of quality of scanning scope 35~450.
5) setting completed for chromatographic quantitative analysis parameter and mass spectrometry analysis condition, after baseline stability, clicks on " RUN ",
Agilent gas chromatograph-mass spectrometer Agilent 6890N-5973I then start automatical analysis detection, Agilent 7693A
16 liquid automatic samplers of Autoinjector start sample introduction, and after the completion of sample introduction, sample introduction needle is repeatedly rinsed using acetone
Wash, until the residual sample in sample introduction needle cleans up completely, analyze by instrument Agilent gas chromatograph-mass spectrometer Agilent
6890N-5973I is completed, and chromatographic quantitative analysis is directly read using area normalization method in instrument interface, and mass spectrometry is analyzed in instrument
The composition at each peak is differentiated in device, therefrom choose adulterated component substances, the instrument can use U.S.'s Agilent makings
Combined instrument Agilent 6890N-5973I.
Acetone, analyzes pure, content 99.5%, and acetone is used for the automatic cleaning of sample introduction needle after the completion of sample introduction, belongs to cleaning agent.
Rosa Damascana technical parameter is as follows：
Color shape：It is viscous liquid at 25 DEG C to be colourless to yellow liquid；
Fragrance：Have the rose aroma of sweet tea rhythm, give off a strong fragrance；
Refraction index (20 DEG C)：1.4520~1.4700；
Relative density (20 DEG C/20 DEG C)：0.8480~0.8800；
Acid number：7~24；
Optical activity (25 DEG C)：- 5 °~-1.8 °；
Main component：Geraniol, nerol, citronellol, benzyl carbinol, linalool, citronellyl acetate etc.；Shelf-life：Packaging
Completely, in the case of without unpacking, 1 year shelf-life；
Condition of storage：In shady and cool, dry, ventilation warehouse, avoid miscellaneous gas from polluting, keep fire away.
Table 1
Rear signal result is as shown in table 1.
Claims (10)
1. the adulterated discrimination method of a kind of natural rose essential, it is characterised in that comprise the following steps：
1) take natural rose essential to be dissolved in absolute ethyl alcohol, after shaking up, draw 1mL injection sample bottles, then be positioned in injector；
2) menu editing is entered from computer for analysis interface, editor, which finishes, presses " preservation " button；
3) chromatographic quantitative analysis parameter is set；
4) mass spectrometry analysis condition is set；
5) setting completed for chromatographic quantitative analysis parameter and mass spectrometry analysis condition, after baseline stability, clicks on " RUN ", makings
Combined instrument then starts automatical analysis detection, and automatic sampler starts sample introduction, and after the completion of sample introduction, sample introduction needle is carried out using acetone
Rinse, until the residual sample in sample introduction needle cleans up completely, analyze and completed by gas chromatograph-mass spectrometer, chromatographic quantitative analysis uses
Area normalization method is directly read at gas chromatograph-mass spectrometer interface, and mass spectrometry analysis is entered in gas chromatograph-mass spectrometer to the composition at each peak
Row differentiates, therefrom chooses adulterated component substances.
2. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 1)
Absolute ethyl alcohol is using the absolute ethyl alcohol for analyzing pure content 99.7%.
3. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 1)
Sample bottle uses 2mL automatic sampler sample bottles.
4. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 1)
Injector is analyzed using automatic sampler, and sample size is 1 μ L；The automatic sampler uses 7693A Autoinjector
16 liquid automatic samplers.
5. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 2)
Into menu editing content of edit include but is not limited to sample ID, model, lot number and sample be placed in corresponding to injector it is empty
Lattice number.
6. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 3)
Chromatographic quantitative analysis parameter is：
Chromatographic column：HP-5MS posts (60m × 0.25mm × 0.25 μm), FID flame ionization ditectors, carrier gas are helium, permanent
Stream mode, flow are 1.0~2.0ml/min, are not shunted；Temperature programming：80 DEG C of initial temperature, 280 are warming up to 4 DEG C/min
DEG C, 5min is kept, rear operation is warming up to 300 DEG C, keeps 5min；Total run time 60min, 280 DEG C of satellite interface temperature.
7. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 4)
Mass spectrometry analysis condition is：
230 DEG C of ion source temperature, 150 DEG C of quadrupole rod temperature, mode EI is ionized, electron energy 70eV, the μ A of heater current 34.6, is swept
Retouch the μ of mass range 35~450.
8. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 5)
Gas chromatograph-mass spectrometer uses U.S. Agilent gas chromatograph-mass spectrometer Agilent 6890N-5973I.
9. the adulterated discrimination method of a kind of natural rose essential as claimed in claim 1, it is characterised in that described in step 5)
Automatic sampler uses 16 liquid automatic samplers of Agilent 7693A Autoinjector.
A kind of 10. adulterated discrimination method of natural rose essential as claimed in claim 1, it is characterised in that in step 5), institute
State acetone and be used for the automatic cleaning of sample introduction needle after the completion of sample introduction using pure, content 99.5%, acetone is analyzed；It is described to rinse using extremely
It is few 2 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711072489.3A CN107621513A (en) | 2017-11-03 | 2017-11-03 | A kind of adulterated discrimination method of natural rose essential |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711072489.3A CN107621513A (en) | 2017-11-03 | 2017-11-03 | A kind of adulterated discrimination method of natural rose essential |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107621513A true CN107621513A (en) | 2018-01-23 |
Family
ID=61093337
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711072489.3A Pending CN107621513A (en) | 2017-11-03 | 2017-11-03 | A kind of adulterated discrimination method of natural rose essential |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107621513A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110412183A (en) * | 2019-09-05 | 2019-11-05 | 中国科学院新疆生态与地理研究所 | A kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104391054A (en) * | 2014-11-08 | 2015-03-04 | 新疆于田瑰觅生物科技股份有限公司 | Standard GC/ MS fingerprint detection method of Hetian Damascus rose essential oil |
| CN105018235A (en) * | 2015-07-21 | 2015-11-04 | 扬州大学 | Method for rapid extracting of rose essential oil from fresh rose flower |
| CN105938129A (en) * | 2016-07-08 | 2016-09-14 | 上海应用技术学院 | Pingyin rose essential oil GC chromatographic method |
-
2017
- 2017-11-03 CN CN201711072489.3A patent/CN107621513A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104391054A (en) * | 2014-11-08 | 2015-03-04 | 新疆于田瑰觅生物科技股份有限公司 | Standard GC/ MS fingerprint detection method of Hetian Damascus rose essential oil |
| CN105018235A (en) * | 2015-07-21 | 2015-11-04 | 扬州大学 | Method for rapid extracting of rose essential oil from fresh rose flower |
| CN105938129A (en) * | 2016-07-08 | 2016-09-14 | 上海应用技术学院 | Pingyin rose essential oil GC chromatographic method |
Non-Patent Citations (6)
| Title |
|---|
| KRASIMIR E. RUSANOV等: "Comparative GC/MS Analysis of Rose Flower and Distilled Oil Volatiles of The Oil Bearing Rose Rosa Damascena", 《BIOTECHNOLOGY & BIOTECHNOLOGICAL EQUIPMENT》 * |
| VELIZAR GOCHEV等: "Comparative Evaluation of Antimicrobial Activity and Composition of Rose Oils From Various Geographic Origins,in Particular Bulgarian Rose Oil", 《NATURAL PRODUCT COMMUNICATIONS》 * |
| 单承莺等: "衢州产玫瑰精油化学成分的GC-MS析", 《江苏农业科学》 * |
| 徐金玉等: "新疆玫瑰精油与保加利亚玫瑰精油化学成分及香气比较", 《冷飲與速凍食品工業》 * |
| 母多等: "玫瑰精油的提取工艺及化学成分的GC-MS 分析研究", 《昆明学院学报》 * |
| 陈秋鹏等: "新疆和田地区大马士革玫瑰精油GC／MS指纹图谱分析", 《新疆中医药》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110412183A (en) * | 2019-09-05 | 2019-11-05 | 中国科学院新疆生态与地理研究所 | A kind of needle trapping-gas chromatography-mass spectrography is to rose aroma analysis of components method |
| CN110412183B (en) * | 2019-09-05 | 2022-04-15 | 中国科学院新疆生态与地理研究所 | Rose fragrance component analysis method by needle capture-gas chromatography-mass spectrometry |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| An et al. | On-site field sampling and analysis of fragrance from living Lavender (Lavandula angustifolia L.) flowers by solid-phase microextraction coupled to gas chromatography and ion-trap mass spectrometry | |
| CN105842378B (en) | The assay method of flavor component in a kind of electronics smoke sol | |
| CN102830196B (en) | Method for detecting quality of tobacco flavor | |
| Dugo et al. | Elucidation of the volatile composition of Marsala wines by using comprehensive two-dimensional gas chromatography | |
| CN106770707B (en) | The screening method of volatile organic matter in a kind of quick-fried pearl of cigarette filter | |
| Del Signore | Chemometric analysis and volatile compounds of traditional balsamic vinegars from Modena | |
| CN101334385B (en) | Aromatic plant volatility organic matter analytical method | |
| CN107085051B (en) | A kind of construction method and discrimination method of Huanghua Pear redwood tree species finger-print | |
| CN104316635A (en) | Method for rapidly identifying flavor and quality of fruits | |
| CN104122358A (en) | Method for measuring volatile fragrance components of electronic cigarette | |
| CN101504395A (en) | Method for controlling quality of flavoring essence for tobacco by gas-phase fingerprint pattern | |
| Biernacka et al. | Volatile composition of raw spirits of different botanical origin | |
| CN106872608A (en) | Limited in a kind of cosmetics with the detection method of anaphylactogen perfume materials | |
| CN109541073A (en) | A kind of francolin congo red, the GC-MS analysis method of green fresh leaf volatile component | |
| CN107621513A (en) | A kind of adulterated discrimination method of natural rose essential | |
| CN103308637B (en) | Gas chromatography-mass spectrometry method for identifying dalbergia odorifera and dalbergia tonkinensi | |
| Qi et al. | Evaluation of orchid-like aroma between different grades of taiping houkui tea by solid-phase microextraction and comprehensive two-dimensional gas chromatography coupled with time-of-fight mass spectrometry | |
| CN108845060A (en) | A kind of method of thermal desorption-gas chromatography/mass spectrometry analysis olive oil volatile flavor component | |
| Xu et al. | Characteristic aroma analysis of finger citron in four different regions based on GC–MS‐HS‐SPME and ROAV | |
| Mehinagic et al. | Optimization of extraction of apple aroma by dynamic headspace and influence of saliva on extraction of volatiles | |
| CN108562668A (en) | A kind of method of GC-MS and tentaculum electric potential instrument combination analysis insect infochemical | |
| CN110082457A (en) | A kind of detection method of Chinese prickly ash pericarp fragrance component | |
| CN106198804A (en) | The authentication method of nitrogen-containing compound in a kind of cherry wine | |
| CN105738505A (en) | Detection method for volatile spice ingredients in coriander | |
| CN110514757A (en) | A kind of method of Volatile flavor components in fast resolving white wine |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180123 |
|
| RJ01 | Rejection of invention patent application after publication |